Formalin Inactivation of Virus for Safe Downstream Processing of Routine Stool Parasite Examination during the COVID-19 Pandemic

✅ 全文

COVID-19大流行期间用于常规粪便寄生虫检查安全下游处理的病毒福尔马林灭活

作者 Pisith Chinabut; Nuntiya Sawangkla; Suphaluck Wattano; Techit Thavorasak; Weluga Bootsongkorn; Anchalee Tungtrongchitr; Pichet Ruenchit 期刊 Diagnostics 发表日期 2023 卷/期/页码 Vol. 13(3) ISSN 2075-4418 DOI 10.3390/diagnostics13030466 类型 原创研究 (Original Research)

📄 英文摘要 English Abstract

EN

During the COVID-19 pandemic, the parasitology laboratories dealing with fecal samples for the diagnosis of gastrointestinal parasitic infections are confronting the unsaved virus-containing samples. To allow for safe downstream processing of the fecal samples, a protocol for preparing a fecal smear is urgently needed. Formalin was tested with or without isotonic forms for virus inactivation using porcine epidemic diarrhea virus (PEDV) as a representative, as it belongs to the Coronaviridae family. The results revealed complete inactivation activity of 10% formalin and 10% isotonic formalin on coronavirus after 5 min of treatment at room temperature. Both also inhibited Naegleria fowleri growth after 5 min of treatment at 37 °C without disruption of the structure. In addition to these key findings, it was also found that isotonic formalin could stabilize both red and white blood cells when used as a solution to prepare fecal smears comparable to the standard method, highlighting its value for use instead of 0.9% normal saline solution for the quantification of blood cells without active virus. The 10% isotonic formalin is useful to safely prepare a fecal smear for the diagnosis of parasites and other infections of the gastrointestinal tract during the COVID-19 pandemic.

📄 中文摘要 Chinese Abstract

中文
在2019冠状病毒病(COVID-19)大流行期间,处理粪便样本用于胃肠道寄生虫感染诊断的寄生虫学实验室面临着含有未灭活病毒样本的安全隐患。为了能够安全地对粪便样本进行下游处理,亟需建立一种粪便涂片制备方案。2020年3月,世界卫生组织(WHO)将COVID-19定性为大流行。该病由严重急性呼吸综合征冠状病毒2型(SARS-CoV-2)引起,与猪流行性腹泻病毒(PEDV)同属冠状病毒科。在40%至85%的中重度COVID-19患者粪便样本中已检测到SARS-CoV-2 RNA,且从粪便样本中也分离出了具有感染性的SARS-CoV-2病毒颗粒。这一证据证实了粪-口或粪-呼吸道传播的潜在风险,并凸显了建立适当粪便标本处理程序的必要性。使用生理盐水(NSS)的简单涂片法是寄生虫感染诊断及红细胞、白细胞计数的常规方法,但生理盐水无法灭活SARS-CoV-2。因此,在COVID-19大流行期间亟需建立一种新的、安全的粪便涂片制备方案。

📋 英文结构化总结 English Structured Summary

全文整理

EN

Background:

During the COVID-19 pandemic, the parasitology laboratories dealing with fecal samples for the diagnosis of gastrointestinal parasitic infections are confronting the unsaved virus-containing samples. To allow for safe downstream processing of the fecal samples, a protocol for preparing a fecal smear is urgently needed. Coronavirus disease of 2019 (COVID-19) was characterized as a pandemic in March 2020 by the World Health Organization (WHO). It is caused by the severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2), a member of the same coronavirus family as the porcine epidemic diarrhea virus (PEDV). SARS-CoV-2 RNA has been detected in 40% to 85% of fecal samples collected from patients with moderate-to-severe COVID-19, and infectious SARS-CoV-2 particle has also been isolated from stool samples. This evidence affirms the potential for fecal–oral or fecal–respiratory transmission and warrants the need for an appropriate handling procedure of fecal specimens. A simple smear technique using normal saline solution (NSS) is the routine method for diagnosis of parasitic infections and enumeration of red and white blood cells, but NSS cannot inactivate SARS-CoV-2. Therefore, a new and saved protocol of fecal smear preparation during the COVID-19 pandemic is urgently needed.

Methods:

Formalin was tested with or without isotonic forms for virus inactivation using porcine epidemic diarrhea virus (PEDV) as a representative, as it belongs to the Coronaviridae family. The results revealed complete inactivation activity of 10% formalin and 10% isotonic formalin on coronavirus after 5 min of treatment at room temperature. Both also inhibited Naegleria fowleri growth after 5 min of treatment at 37 °C without disruption of the structure. In addition to these key findings, it was also found that isotonic formalin could stabilize both red and white blood cells when used as a solution to prepare fecal smears comparable to the standard method.

Results:

The results revealed complete inactivation activity of 10% formalin and 10% isotonic formalin on coronavirus after 5 min of treatment at room temperature. Both also inhibited Naegleria fowleri growth after 5 min of treatment at 37 °C without disruption of the structure. In addition to these key findings, it was also found that isotonic formalin could stabilize both red and white blood cells when used as a solution to prepare fecal smears comparable to the standard method, highlighting its value for use instead of 0.9% normal saline solution for the quantification of blood cells without active virus.

Data Summary:

Complete inactivation activity of 10% formalin and 10% isotonic formalin on coronavirus was achieved after 5 min of treatment at room temperature. Inhibition of Naegleria fowleri growth occurred after 5 min of treatment at 37 °C. Isotonic formalin stabilized both red and white blood cells, comparable to the standard method using 0.9% normal saline solution.

Conclusions:

The 10% isotonic formalin is useful to safely prepare a fecal smear for the diagnosis of parasites and other infections of the gastrointestinal tract during the COVID-19 pandemic.

Practical Significance:

Isotonic formalin can be used instead of 0.9% normal saline solution for the quantification of blood cells without active virus, enabling safe downstream processing of fecal samples for laboratory personnel during the COVID-19 pandemic.

📋 中文结构化总结 Chinese Structured Summary

中文

背景:

在2019冠状病毒病(COVID-19)大流行期间,处理粪便样本用于胃肠道寄生虫感染诊断的寄生虫学实验室面临着含有未灭活病毒样本的安全隐患。为了能够安全地对粪便样本进行下游处理,亟需建立一种粪便涂片制备方案。2020年3月,世界卫生组织(WHO)将COVID-19定性为大流行。该病由严重急性呼吸综合征冠状病毒2型(SARS-CoV-2)引起,与猪流行性腹泻病毒(PEDV)同属冠状病毒科。在40%至85%的中重度COVID-19患者粪便样本中已检测到SARS-CoV-2 RNA,且从粪便样本中也分离出了具有感染性的SARS-CoV-2病毒颗粒。这一证据证实了粪-口或粪-呼吸道传播的潜在风险,并凸显了建立适当粪便标本处理程序的必要性。使用生理盐水(NSS)的简单涂片法是寄生虫感染诊断及红细胞、白细胞计数的常规方法,但生理盐水无法灭活SARS-CoV-2。因此,在COVID-19大流行期间亟需建立一种新的、安全的粪便涂片制备方案。

方法:

以猪流行性腹泻病毒(PEDV)作为冠状病毒科的代表,测试了福尔马林及其等渗形式对病毒的灭活效果。结果显示,10%福尔马林和10%等渗福尔马林在室温下处理5分钟后对冠状病毒均表现出完全的灭活活性。两者在37°C下处理5分钟后均能抑制福氏耐格里阿米巴(Naegleria fowleri)的生长,且不破坏其结构。除上述关键发现外,研究还发现等渗福尔马林作为粪便涂片制备溶液时,能够稳定红细胞和白细胞,其效果与标准方法相当。

结果:

结果显示,10%福尔马林和10%等渗福尔马林在室温下处理5分钟后对冠状病毒均表现出完全的灭活活性。两者在37°C下处理5分钟后均能抑制福氏耐格里阿米巴的生长,且不破坏其结构。除上述关键发现外,研究还发现等渗福尔马林能够稳定红细胞和白细胞,其效果与使用0.9%生理盐水的标准方法相当,凸显了其替代0.9%生理盐水用于无活性病毒状态下血细胞定量的应用价值。

数据总结:

10%福尔马林和10%等渗福尔马林在室温下处理5分钟后实现了对冠状病毒的完全灭活。在37°C下处理5分钟后可抑制福氏耐格里阿米巴的生长。等渗福尔马林能够稳定红细胞和白细胞,其效果与使用0.9%生理盐水的标准方法相当。

结论:

10%等渗福尔马林可用于在COVID-19大流行期间安全制备粪便涂片,以诊断寄生虫及胃肠道其他感染。

实际意义:

等渗福尔马林可替代0.9%生理盐水用于无活性病毒状态下的血细胞定量,使实验室人员能够在COVID-19大流行期间安全地对粪便样本进行下游处理。

📖 英文全文 English Full Text

EN

Diagnostics 2023, 13, 466. https://doi.org/10.3390/diagnostics13030466 www.mdpi.com/journal/diagnostics

Article Formalin Inactivation of Virus for Safe Downstream Processing of Routine Stool Parasite Examination during the COVID-19

Pandemic Pisith Chinabut 1, Nuntiya Sawangkla 1, Suphaluck Wattano 1, Techit Thavorasak 2, Weluga Bootsongkorn 3,

Anchalee Tungtrongchitr 1 and Pichet Ruenchit 1,3,*

1 Department of Parasitology, Faculty of Medicine Siriraj Hospital, Mahidol University,

Bangkok 10700, Thailand 2 Center of Research Excellence in Therapeutic Proteins and Antibody Engineering, Department of

Parasitology, Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok 10700, Thailand

3 Siriraj Integrative Center for Neglected Parasitic Diseases, Department of Parasitology, Faculty of Medicine

Siriraj Hospital, Mahidol University, Bangkok 10700, Thailand

* Correspondence: pichet.rue@mahidol.edu; Tel.: +66-24196484

Abstract: During the COVID-19 pandemic, the parasitology laboratories dealing with fecal samples for the diagnosis of gastrointestinal parasitic infections are confronting the unsaved virus-contain- ing samples. To allow for safe downstream processing of the fecal samples, a protocol for preparing a fecal smear is urgently needed. Formalin was tested with or without isotonic forms for virus inac- tivation using porcine epidemic diarrhea virus (PEDV) as a representative, as it belongs to the Coro- naviridae family. The results revealed complete inactivation activity of 10% formalin and 10% iso- tonic formalin on coronavirus after 5 min of treatment at room temperature. Both also inhibited

Naegleria fowleri growth after 5 min of treatment at 37 °C without disruption of the structure. In addition to these key findings, it was also found that isotonic formalin could stabilize both red and white blood cells when used as a solution to prepare fecal smears comparable to the standard method, highlighting its value for use instead of 0.9% normal saline solution for the quantification of blood cells without active virus. The 10% isotonic formalin is useful to safely prepare a fecal smear for the diagnosis of parasites and other infections of the gastrointestinal tract during the

COVID-19 pandemic.

Keywords: COVID-19; formalin; inactivation; infectious diseases; isotonic formalin; normal saline solution; red blood cell; stool examination; white blood cell

1. Introduction Coronavirus disease of 2019 (COVID-19) was characterized as a pandemic in March

2020 by the World Health Organization (WHO) [1]. It is caused by the severe acute res- piratory syndrome coronavirus 2 (SARS-CoV-2), a member of the same coronavirus fam- ily as the Middle East respiratory syndrome coronavirus (MERS-CoV), porcine epidemic diarrhea virus (PEDV), etc. [2]. As of December 2022, more than 600 million people have been infected with SARS-CoV-2 and nearly seven million infected people have died [3].

The virus spreads mainly between people through small liquid particles secreted from the mouth or nose by coughing, sneezing, breathing, speaking or singing, and human-to-hu- man contact [4].

Fever, dry cough, and dyspnea are the most common manifestations of COVID-19, while diarrhea, nausea, vomiting, and abdominal discomfort are the less common features [5]. In addition to nasal and saliva samples, SARS-CoV-2 has been reported to be isolated from the urine of a patient with severe COVID-19 [6]. Furthermore, the shedding of the

Citation: Chinabut, P.; Sawangkla, N.; Wattano, S.; Thavorasak, T.;

Bootsongkorn, W.; Tungtrongchitr, A.; Ruenchit, P. Formalin

Inactivation of Virus for Safe Downstream Processing of Routine

Stool Parasite Examination during the COVID-19 Pandemic.

Diagnostics 2023, 13, 466. https://doi.org/10.3390/ diagnostics13030466

Academic Editors: Philippe Colson and Francesco Inchingolo

Received: 5 January 2023 Revised: 20 January 2023 Accepted: 25 January 2023

Published: 27 January 2023

Copyright: © 2023 by the authors.

Licensee MDPI, Basel, Switzerland.

This article is an open access article distributed under the terms and conditions of the Creative Commons

Attribution (CC BY) license (https://creativecommons.org/license s/by/4.0/).

Diagnostics 2023, 13, 466 2 of 11

virus in feces has been documented. SARS-CoV-2 RNA has been detected in 40% to 85% of fecal samples collected from patients with moderate-to-severe COVID-19 [7–9]. The in- fectious SARS-CoV-2 particle has also been isolated from stool samples from COVID-19 patients [10], and stool samples collected from patients with gastrointestinal manifesta- tions [11]. The shedding of SARS-CoV-2 RNA in feces was found to be correlated with gastrointestinal symptoms [12]. Half of the COVID-19 patients with mild to moderate symptoms shed fecal SARS-CoV-2 RNA within the first week after diagnosis. Thirteen percent of the patients continued to shed viral RNA in their feces 4 months after diagnosis, while nearly 4% shed at 7 months [12]. Interestingly, rectal swabs from eight out of ten pediatric cases of COVID-19 were found to persistently test positive for COVID-19 by real- time reverse transcription—polymerase chain reaction (RT–PCR) even after nasopharyn- geal testing was negative [13]. This evidence affirms the potential for fecal–oral or fecal– respiratory transmission and warrants the need for an appropriate handling procedure of fecal specimens collected from suspected or confirmed cases of COVID-19 in order to avoid the possible transmission of SARS-CoV-2 from feces.

During the COVID-19 pandemic, diagnostic laboratories, including the parasitology laboratory, are confronted with unreliable viral inactivation and safety of clinical speci- mens. The parasitology laboratory must deal with fecal samples to diagnose gastrointes- tinal parasitic infections, as well as quantification of red and white blood cells in order to evaluate other infections in the gastrointestinal tract. A simple smear technique or direct wet smear is a basic, conventional, gold standard, and the routine method for the diagno- sis of parasitic infections by detecting ova and parasites in stool samples under the micro- scope [14]. On the basis of this technique, normal saline solution (NSS) containing 0.9% sodium chloride is normally used as a solution to prepare a fecal smear. This concentra- tion showed an osmolarity equal to that of blood plasma, indicating its ability to stabilize red and white blood cells shed in fecal samples [15]. Therefore, it is a good choice and was selected to prepare the fecal smears for enumeration of red and white blood cells. How- ever, this solution cannot inactivate SARS-CoV-2, which can be contaminated in the feces.

Therefore, to allow safe downstream processing of fecal samples for laboratory personnel, a new and saved protocol of fecal smear preparation during the COVID-19 pandemic is urgently needed.

Recently, various detergents and chaotropic reagents were shown to completely in- activate SARS-CoV-2 and other coronaviruses, such as 4% sodium dodecyl sulphate (SDS), 1% sodium deoxycholate (SDC), and trifluoroacetic acid (TFA) in a 1:4 ratio, while

6M guanidinium chloride (GdmCl) and 8M urea partially inactivate [16]. Chlorhexidine digluconate, anionic surfactant, and calcium bicarbonate with a mesoscopic structure (CAC-717) were also found to exhibit virucidal activity against SARS-CoV-2 [17]. Forma- lin is another chemical agent that is used to inactivate many types of viruses, such as in- fluenza A virus, adenovirus, cytomegalovirus, hepatitis A virus, and poliovirus [18–20].

It reacts with amino acids of target viral proteins acting on the N-terminal amino group and side-chains of arginine, cysteine, histidine, and lysine residues to form reversible methylol adducts and nonreversible methylene bridges [21]. However, formalin inactiva- tion activity against coronaviruses and its application to stool examination for the safety of coronavirus transmission through fecal specimens has not been studied extensively.

Therefore, the objective of the present study is to evaluate the inactivation activity of for- malin against coronavirus, using PEDV as the representative, and its effectiveness in red and white blood cells analyses. The results of the present study will suggest suitable meth- ods for handling SARS-CoV-2-containing fecal specimens. Additionally, it is possible to note that this unexpected material could be handled in a laboratory setting of standard biosafety level-2 (BSL-2).

Diagnostics 2023, 13, 466 3 of 11

2. Materials and Methods 2.1. Human Ethics Human ethics was reviewed and exempted by the Siriraj Institutional Review Board of the Faculty of Medicine Siriraj Hospital, Mahidol University, Thailand (SIRB Protocol

No. 499/2564) because the samples used in this study were not collected directly from patients.

2.2. Microorganisms and Cell Line Porcine epidemic diarrhea virus (PEDV) P70 strain, a coronavirus that does not pose a risk to human health and can be handled in a biosafety level-2 (BSL-2) laboratory, and

Naegleria fowleri CDC VO 3081 strain, a free-living parasite that can be easily cultured, were used as representatives to test for chemical inactivation by formalin. The African green monkey kidney cell (Vero) was used for the propagation of PEDV. The PEDV and

Vero cell line were obtained from Emeritus Professor Dr. Wanpen Chaicumpa at the Cen- ter of Research Excellence in Therapeutic Proteins and Antibody Engineering. N. fowleri was obtained from Dr. GS Visvesvara at the Centers for Disease Control and Prevention (USCDC).

2.3. Chemical Agents The normal saline solution (NSS) at 0.9% (w/v) of sodium chloride (NaCl) was from

Thai Nakorn Patana Co., Ltd. 10% formalin was prepared by mixing 100 mL of formalde- hyde solution (KEMAUS, Bangkok, Thailand) with 1 L of sterile distilled water. Isotonic formalin (10%; v/v) was prepared by dissolving 0.9 g of NaCl in 10% formalin.

2.4. Propagation of Porcine Epidemic Diarrhea Virus

PEDV was propagated in African green monkey kidney cell (Vero). Briefly, Vero cells were grown in Dulbecco’s modified Eagle’s medium (DMEM) (Gibco, Life Technologies

Corporation, Grand Island, NY, USA) supplemented with 10% heat-inactivated fetal bo- vine serum (FBS; HyClone, GE Healthcare Bio-Sciences Austria GmbH, Pasching, Aus- tria), 2 mM L-alanyl-L-glutaminase dipeptide (Gibco, Life Technologies Corporation,

Grand Island, NY, USA), 100 UmL−1 penicillin (Gibco, Life Technologies Corporation,

Grand Island, NY, USA), and 100 µgmL−1 streptomycin (Gibco, Life Technologies Corpo- ration, Grand Island, NY, USA). The cells were cultured at 37 °C in a humidified incubator with 5% CO2. Then, cells were collected and washed twice with sterile phosphate buffered saline (PBS), pH 7.4, and transfected with PEDV at MOI 0.001. The virus was kept at 37 °C in a humidified incubator with 5% CO2 until use.

2.5. Cultivation of Naegleria fowleri N. fowleri was grown in Nelson’s medium supplemented with 10% FBS at 37 °C in a

T 25 cm2 flask (Corning, New York, NY, USA) in a secure facility.

2.6. In Vitro Inactivation of Coronavirus and Plaque Formation Assay

To test whether a coronavirus could be inactivated with 10% formalin or 10% isotonic formalin, a plaque formation assay was performed using the PEDV P70 strain as the rep- resentative [22]. Briefly, 100 µL of 10% formalin or 10% isotonic formalin were mixed with

100 µL of PEDV aliquots (178,000 pfu) and incubated at room temperature for 5 min. After dilution with DMEM at 1:10,000, 1 mL of each of the mixtures were then added to separate wells (triplicate) of 24-well tissue culture plates containing a confluent monolayer of Vero cells and incubated at 37 °C in a humidified incubator with 5% CO2 for an hour to allow virus attachment to cells. Virus in medium alone and noninfected Vero cells (mock) were used as negative inactivation control and negative plaque formation control, respectively.

The free PEDV particles were removed, and the cells were washed twice with PBS. Car- boxymethyl cellulose (CMC) (2% CMC in DMEM supplemented with 2 µgmL−1 of TPCK

Diagnostics 2023, 13, 466 4 of 11

treated trypsin) was added to each well. The plates were incubated at 37 °C in a humidi- fied incubator with 5% CO2 for 48 h. Cells were fixed with 10% formalin at room temper- ature for 1 h before staining with 1% crystal violet dye in 10% ethanol. The inactivation of

PEDV was observed by the absence of plaque formation in Vero cells. The number of plaques was counted by light microscopy at 40× magnification.

2.7. Inactivation of Parasite To evaluate the inactivation activity of 10% formalin and 10% isotonic formalin against parasites, N. fowleri (a free-living amoeba) was selected as a representative for test- ing. Logarithmic phase N. fowleri trophozoites (1 × 104 cells) in 100 µL of Nelson’s medium supplemented with 10% FBS, 100 UmL−1 penicillin, and 100 µgmL−1 streptomycin were seeded in individual wells of 96-well tissue culture plates, and incubated at 37 °C for 24 h. After discarding the culture medium, 100 µL of 10, 5, and 2.5% formalin and isotonic formalin were added to the wells containing the amoebae. The amoebae wells with me- dium alone served as a negative inactivation control, while the amoebae wells with 0.9%

NSS served as a positive inactivation control. The plates were kept at 37 °C for 5 min. The number of viable amoebae in each treatment was determined using the CellTiter-Glo® 3D

Cell Viability Assay (Promega, Promega Corporation, Madison, WI, USA). The percentage of trophozoite survival was calculated as follows: [(luminous intensity of the test sam- ple/luminous intensity of the negative inactivation control sample)] × 100. Results are shown as mean ± standard deviation (SD) of a representative of 3 independent experi- ments.

2.8. Preparation of Fecal Smear Fecal smears were prepared using 3 reagents, 0.9% NSS (a standard solution), 10% formalin, and 10% isotonic formalin (as developed in this study) [23]. Briefly, a drop of stool sample was thoroughly mixed with a drop of 0.9% NSS, 10% formalin, or 10% iso- tonic formalin on a glass slide, smeared as a thin film, covered with a glass cover slip, and left at room temperature for 5, 10, 20, and 30 min. All experiments were performed under the class II biological safety cabinet in the BSL-2 laboratory in the Department of Parasit- ology of the Faculty of Medicine Siriraj Hospital, Mahidol university.

2.9. Examination of Parasite The fecal smears prepared with 0.9% NSS, 10% formalin, and 10% isotonic formalin were investigated for ova and parasites under a microscope at 400× magnification.

2.10. Enumeration of Red and White Blood Cells The numbers of red blood cells (RBC) and white blood cells (WBC) presented in each fecal smear prepared above were counted under microscope at 400× magnification, and grouped into the ranges of 0–1, 2–3, 4–5, 6–10, 11–20, 21–30, 31–50, and >50 Cells/High Dry (HD). The counting step was performed by the three independent laboratory technicians.

The number of RBC and WBC detected in the smears were shown as percentages. The results of two methods (fecal smears prepared using 0.9% NSS and 10% isotonic formalin) were compared.

2.11. Statistical Analysis The measurement of agreement between the two methods (fecal smears prepared with 10% isotonic formalin and 0.9% NSS) and inter-rater reliability among the three la- boratory technicians were evaluated using IBM SPSS Statistics for Windows, version 21 (IBM Corp., Armonk, NY, USA) and shown as the Kappa coefficient and the Fleiss kappa value in a 95% confidence interval (CI), respectively. The results were considered signifi- cantly different at p-value < 0.05.

Diagnostics 2023, 13, 466 5 of 11

3. Results and Discussion 3.1. Inactivation Activiy of Formalin against Coronavirus

To test the inactivation activity of formalin to porcine epidemic diarrhea virus, a rep- resentative of coronaviruses, PEDV was treated in vitro with 10% formalin and 10% iso- tonic formalin at room temperature for 5 min. Viability of viruses was evaluated using a plaque formation assay using Vero cells as the host (Figure 1a). PEDV was found to be completely inactivated by 10% formalin and 10% isotonic formalin after 5 min of treat- ment. Plaque formation was not detected in PEDV treated with 10% formalin or 10% iso- tonic formalin, while it was observed in untreated PEDV as shown in Figure 1b. This data indicated that PEDV, a species of coronaviruses, could be neutralized with formalin in a short period (5 min). Previously, it has been reported that PEDV was susceptible to 4% anhydrous sodium carbonate, 1% iodophores in phosphoric acid, and 2% sodium hydrox- ide [24]. Even though 1% formalin has been reported to inactivate PEDV [24], the isotonic form of this agent has not been studied. This study reported for the first time about inac- tivation activity of isotonic formalin to PEDV. In terms of duration of action, findings of the present study are consistent with previous studies showing that SARS-CoV-2 was completely inactivated by Trizol and Trizol LS (1:4 virus:Trizol reagent) at room temper- ature for 5 min [25]. Meanwhile, 0.5% SDS, 0.5% Triton X-100, 0.5% NP-40, 100% methanol, and 4% paraformaldehyde were also shown to neutralize SARS-CoV-2 at room tempera- ture, but required a longer duration of treatment (30 min) [25]. Since PEDV and SARS- Cov-2 are viruses in the same family and shared some similar biochemical and biological properties, such as the membrane fusion processes, global folding of M protein, etc. [2,26], sensitivity of these viruses to formalin may be the same. Therefore, 10% formalin and 10% isotonic formalin are good candidates to be used as virus-inactivating agents in laborato- ries that perform downstream work on samples that contain SARS-CoV-2.

Figure 1. Inactivation activities of 10% formalin and 10% isotonic formalin on porcine epidemic di- arrhea virus (PEDV): (a) Flow diagram of in vitro inactivation assay. (b) Number of plaques per well of 10% formalin- and 10% isotonic formalin-treated PEDV at 5 min of treatment at room tempera- ture. Virus in medium alone and noninfected Vero cells (mock) were used as a negative inactivation control and a negative plaque formation control, respectively. The results are shown as the mean ± standard deviation (SD) of a representative of three independent experiments.

Diagnostics 2023, 13, 466 6 of 11

3.2. Formalin Inactivation of Free-Living Parasite

To test the ability of formalin to inactivate the parasite, N. fowleri, which is a free- living amoeba that causes primary amoebic meningoencephalitis in humans by invading the nostrils through water or dust contaminated with the parasite [27], was tested for in vitro inhibition by formalin and isotonic formalin at different concentrations. Parasite vi- ability was evaluated using the CellTiter-Glo® 3D Cell Viability Assay, which accurately measured cell viability based on the quantitation of adenosine triphosphate (ATP) (Figure

2a) [28]. It was found that all concentrations (10, 5, and 2.5%) of formalin and isotonic formalin completely inactivated the parasite after 5 min of treatment at 37 °C, while the untreated parasite was alive (Figure 2b). This result is in accordance with the previous study, which reported that Toxoplasma oocysts were killed by 10% formalin at room tem- perature, but four days of treatment were required [29]. Similarly, Leishmania major pro- mastigotes were also killed by 0.1% formalin, but with an overnight time of treatment required [30]. As expected, 0.9% NSS also inhibited the growth of N. fowleri, since it is a well-known low salinity tolerant organism. The growth of Naegleria spp. has been re- ported to be inhibited under 0.2% NaCl conditions [31]. In the present study, it was found that although N. fowleri was completely inactivated, its morphology was still intact (data not shown). To confirm this evidence, a stool sample was then sampled to prepare the fecal smears using 10% formalin and 10% isotonic formalin, and the ova and parasites were investigated. The presence of ova and parasites was compared with that found in the smear prepared by the standard method. Based on this test, the vacuolar form of Blas- tocytis spp. found in a fecal smear prepared with 0.9% NSS was also observed in smears prepared with 10% formalin and 10% isotonic formalin. However, its vacuole appears to be more distinctive in a smear prepared with 0.9% NSS and 10% isotonic formalin (Figure

3). Therefore, it could be concluded that, in addition to coronaviruses, formalin also showed inactivation activity against a parasite and still preserved the morphology of the parasite, which will be beneficial for the examination of stool. It is not surprising that for- malin maintained the structure of the parasite, because it is a well-known fixative agent used most often for newly obtained samples, including stool samples. It stabilized the biological structure by penetrating the sample, binding to amino acids in all proteins, re- acting to uncharged reactive amino groups, and causing cross-links [32]. However, it should be noted that formalin is not suitable for the diagnosis of parasites whose motility is needed for the diagnosis.

Diagnostics 2023, 13, 466 7 of 11

Figure 2. Inactivation activities of formalin and isotonic formalin at different concentrations against

Naegleria fowleri: (a) Flow diagram of inactivation assay. (b) Percent survival of N. fowleri trophozo- ites treated with formalin and isotonic formalin 5 min at 37 °C. The results are shown as the mean ± standard deviation (SD) of a representative of three independent experiments.

Figure 3. Presence of parasite in the fecal smears. Fecal smears were prepared using different solu- tions, including 0.9% normal saline solution (NSS) (left), 10% formalin (middle), and 10% isotonic formalin (right). Ova and parasites were observed. One block of scale bar represents 0.25 microme- ters. The red arrow indicates the vacuolar form of Blastocystis spp. The lower right corner of each figure displays a zoomed-in image of the vacuolar form.

3.3. Use of Formalin to Prepare Fecal Smears for the Analysis of Red and White Blood Cells

In addition to investigating ova and parasites, the Parasitology laboratory also enu- merated red and white blood cells presented in fecal samples to evaluate other infections in the gastrointestinal tract. Since 10% formalin and 10% isotonic formalin showed inacti- vation activity for both a coronavirus and a parasite, it would be worth if it could also be used to prepare a fecal smear for the enumeration of RBC and WBC to diagnose other infections in the gastrointestinal tract. To test this, 10% formalin and 10% isotonic formalin were applied to prepare fecal smears and tested for stabilization of both RBC and WBC (Figure 4a). The results showed that 10% formalin could not maintain the RBC found in fecal samples (Figure 4b). Lysis of RBC was found when 10% formalin was used to prepare the fecal smears. Contrarily, both RBC and WBC could be stabilized in fecal smears pre- pared with 10% isotonic formalin or 0.9% NSS, a standard solution, at 0 and 30 min after

Diagnostics 2023, 13, 466 8 of 11

preparation (Figure 4b). This evidence supports the use of 10% isotonic formalin for the preparation of fecal smears because of its ability to stabilize RBC and WBC, and its inacti- vation activity against the coronavirus.

Figure 4. Stabilization of 10% formalin and 10% isotonic formalin blood cells at 0 and 30 min: (a)

Flow diagram of fecal smear preparation and analysis of blood cells. (b) Persistence of red and white blood cells in fecal smears prepared with 10% formalin and 10% isotonic formalin compared to that prepared with 0.9% normal saline solution (NSS), a standard solution. One block of scale bar repre- sents 0.25 micrometers. Red arrow indicates red blood cell (RBC). Green arrow indicates white blood cell (WBC). The upper right and left corners of each figure display zoomed-in images of white and red blood cells, respectively.

To demonstrate the capacity to use 10% isotonic formalin for the quantitative evalu- ation of RBC and WBC using a fecal smear method, 59 stool samples in which RBC or

WBC were detected by the standard method (the fecal smears prepared with 0.9% NSS) were used to prepared fecal smears using 10% isotonic formalin. Both RBC and WBC were found to also be detected in all fecal smears prepared using 10% isotonic formalin. Most fecal smears (27.1 and 25.4%) contain RBC and WBC at more than 50 cells per high dry (cells/HD) (Table 1).

Table 1. Number (Percentage) of the fecal smear samples prepared using 10% isotonic formalin in which RBC and WBC were detected at different numbers (Cells/HD) (n = 59).

Number of Blood Cells (Cells/HD 1) Red Blood Cell Number (Percentage)

White Blood Cell Number (Percentage) 0–1 7 (11.9) 12 (20.3)

2–3 10 (16.9) 11 (18.6) 4–5 7 (11.9) 9 (15.3) 6–10

5 (8.5) 6 (10.2) 11–20 2 (3.4) 4 (6.8) Diagnostics 2023, 13, 466

9 of 11

21–30 11 (18.6) 2 (3.4) 31–50 1 (1.7) ND 2 >50 16 (27.1)

15 (25.4) Total 59 (100.0) 59 (100.0) 1 High Dry. 2 Not detected.

Furthermore, it was found that the numbers of blood cells found in 10% isotonic for- malin prepared fecal smears were similar to that found in the 0.9% NSS prepared fecal smears in all defined cell ranges and time intervals (Kappa coefficient value at 1.00) (Table

2). The consistency of the interpretation results between the two methods was also high (100%) at all time intervals (Table 2). These data indicated that 10% isotonic formalin is a good stabilizer of blood cells present in the fecal smears.

Table 2. Measurement of RBC and WBC agreement between fecal smears prepared with 10% iso- tonic formalin and standard method (the fecal smears prepared with 0.9% NSS) at different time intervals (n = 59).

Time (Min) Kappa Coefficient Value Concordance of Reliable Data p-Value

5 1.00 59 (100%) <0.001 1 10 1.00 59 (100%) <0.001 1

20 1.00 59 (100%) <0.001 1 30 1.00 59 (100%) <0.001 1

1 Significantly different at p-value < 0.05.

To assess the reliability of the agreement of the enumeration of blood cells between the technicians, the three technicians independently performed the enumeration of RBC and WBC in fecal smears prepared with 10% isotonic formalin or 0.9% NSS (Figure 3a).

The numbers of positive blood cell samples were not different (Fleiss kappa value 0.918 and 0.932 for RBC and WBC, respectively) (Table 3).

Table 3. Reliability of agreement (inter-rater reliability) of blood cell enumeration among the three independent technicians.

Number of Blood Cells Fleiss Kappa Value (95% CI) p-Value

RBC 0.918 (0.852–0.983) <0.001 1 WBC 0.932 (0.865–0.998)

<0.001 1 1 Significantly different at p-value < 0.05.

This study confirms the safe use of 10% isotonic formalin for the complete inactiva- tion of the porcine epidemic diarrhea virus in vitro. This agent is likely to be effective against all coronaviruses, especially the SARS-CoV-2, due to their similar biochemical and biological properties. Furthermore, 10% isotonic formalin also inactivated N. fowleri, a rep- resentative of parasites, without any destruction of their structures. Likewise, it also showed its ability to preserve red and white blood cells, indicating application to RBC and

WBC analysis for the diagnosis of other pathogen infections. This evidence may provide guidance for safe laboratory practice in all clinical and research laboratories that handle biological specimens that may contain SARS-CoV-2. However, the formalin hazard re- mains a concern, even though it can be significantly reduced by using masks and special ventilation systems [33].

4. Conclusions For the preparation of a fecal smear for the diagnosis of parasitic infections and the detection of RBC and WBC for the investigation of other gastrointestinal tract infections during the COVID-19 pandemic, 10% isotonic formalin can be applied instead of 0.9%

NSS to ensure the safety of the downstream process in routine stool examination. It not only disinfects coronavirus and the parasite, but also stabilizes the red and white blood

Diagnostics 2023, 13, 466 10 of 11

cells present in the fecal smears. Therefore, 10% isotonic formalin can be used for the prep- aration of fecal smears to ensure that laboratory personnel will be safe while working during the COVID-19 pandemic.

Author Contributions: Conceptualization, A.T., P.C., and P.R.; methodology, A.T., P.C., and P.R.; formal analysis, P.C. and P.R.; investigation, N.S., P.C., S.W., T.T., and W.B.; resources, P.C. and

P.R.; data curation, P.C. and P.R.; writing—original draft preparation, P.C.; writing—review and editing, A.T. and P.R.; visualization, P.C., P.R., T.T., and W.B.; supervision, A.T. and P.R.; project administration, P.C.; funding acquisition, P.C. All authors have read and agreed to the published version of the manuscript.

Funding: This research was funded by Siriraj Research Development Fund (Managed by Routine to Research: R2R), Faculty of Medicine Siriraj Hospital, Mahidol University, Bangkok, Thailand, grant number R016435049. AT and PR are scholars of the “Chalermphrakiat” grants, Faculty of

Medicine Siriraj Hospital, Mahidol University.

Institutional Review Board Statement: Ethical review and approval were waived for this study because all fecal specimens used in the present study were collected from laboratory stocks.

Informed Consent Statement: Not applicable.

Data Availability Statement: Not applicable.

Acknowledgments: The authors gratefully acknowledge Nerisa Thornsri at the Division of Clinical

Epidemiology, Department of Research, Faculty of Medicine Siriraj Hospital, Mahidol University,

Bangkok, Thailand, for supporting the statistical analyses. We offer special thanks to Associate Pro- fessor Pitipol Choopong at Routine to Research Unit and Associate Professor Nitat Sookrung at Bi- omedical Research Incubator Unit, Department of Research, Faculty of Medicine Siriraj Hospital,

Mahidol University, for technical support. Thanks also goes to all staff at the Department of Para- sitology, Faculty of Medicine Siriraj Hospital, Mahidol University.

Conflicts of Interest: The authors declare no conflicts of interest.

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文章 甲醛灭活病毒用于COVID-19疫情期间常规粪便寄生虫检查的安全下游处理

Pisith Chinabut¹, Nuntiya Sawangkla¹, Suphaluck Wattano¹, Techit Thavorasak², Weluga Bootsongkorn³, Anchalee Tungtrongchitr¹ 和 Pichet Ruenchit¹,³,*

¹ 泰国曼谷10700,玛希隆大学诗里拉吉医院医学院寄生虫学系 ² 泰国曼谷10700,玛希隆大学诗里拉吉医院医学院治疗性蛋白与抗体工程研究中心,寄生虫学系 ³ 泰国曼谷10700,玛希隆大学诗里拉吉医院医学院被忽视寄生虫病综合中心,寄生虫学系 * 通信作者:pichet.rue@mahidol.edu;电话:+66-24196484

摘要:在COVID-19疫情期间,处理粪便样本以诊断胃肠道寄生虫感染的寄生虫学实验室面临含有未灭活病毒样本的安全挑战。为安全处理粪便样本,亟需建立一种制备粪便涂片的方案。本研究以猪流行性腹泻病毒(PEDV)作为冠状病毒科的代表,测试了甲醛及其等渗形式对病毒的灭活效果。结果显示,10%甲醛和10%等渗甲醛在室温下处理5分钟即可完全灭活冠状病毒。两者在37°C下处理5分钟内亦能抑制耐格里阿米巴(Naegleria fowleri)的生长,且未破坏其结构。此外,研究发现等渗甲醛在制备粪便涂片时可稳定红细胞和白细胞,效果与标准方法相当,表明其可替代0.9%生理盐水用于无活病毒状态下血细胞的定量分析。10%等渗甲醛可用于在COVID-19疫情期间安全制备粪便涂片,以诊断寄生虫及其他胃肠道感染。

关键词:COVID-19;甲醛;灭活;传染病;等渗甲醛;生理盐水;红细胞;粪便检查;白细胞

1. 引言 2019冠状病毒病(COVID-19)于2020年3月被世界卫生组织(WHO)定性为大流行[1]。其病原体为严重急性呼吸综合征冠状病毒2(SARS-CoV-2),与中东呼吸综合征冠状病毒(MERS-CoV)、猪流行性腹泻病毒(PEDV)等同属冠状病毒科[2]。截至2022年12月,全球已有超过6亿人感染SARS-CoV-2,近700万人因此死亡[3]。该病毒主要通过咳嗽、打喷嚏、呼吸、说话或唱歌时从口鼻排出的小液粒在人际间传播,也可通过人与人接触传播[4]。

发热、干咳和呼吸困难是COVID-19最常见的临床表现,而腹泻、恶心、呕吐和腹部不适则较少见[5]。除鼻咽和唾液样本外,已有报道从重症COVID-19患者的尿液中分离出SARS-CoV-2[6]。此外,粪便中亦存在病毒脱落现象。在40%至85%的中重度COVID-19患者粪便样本中检测到SARS-CoV-2 RNA[7–9]。同时,已从COVID-19患者[10]及有胃肠道症状患者[11]的粪便样本中分离出具有传染性的SARS-CoV-2颗粒。粪便中SARS-CoV-2 RNA的脱落与胃肠道症状相关[12]。半数轻中度症状患者在确诊后第一周内粪便中即可检出SARS-CoV-2 RNA;13%的患者在确诊4个月后仍持续排毒,近4%甚至在7个月后仍可检出[12]。值得注意的是,在10例儿童COVID-19病例中,有8例在鼻咽拭子检测转阴后,直肠拭子经实时逆转录-聚合酶链反应(RT–PCR)仍持续呈阳性[13]。上述证据证实了粪-口或粪-呼吸道传播的可能性,并强调必须对疑似或确诊COVID-19患者的粪便标本采取适当处理程序,以避免SARS-CoV-2通过粪便传播。

在COVID-19疫情期间,包括寄生虫学实验室在内的诊断实验室面临临床标本病毒灭活不可靠及生物安全性的挑战。寄生虫学实验室需处理粪便样本以诊断胃肠道寄生虫感染,并定量检测红细胞和白细胞以评估其他胃肠道感染。直接涂片法或湿片法是诊断寄生虫感染的基本、常规、金标准方法,通过显微镜检查粪便样本中的虫卵和寄生虫[14]。该方法通常使用含0.9%氯化钠的生理盐水(NSS)作为制备粪便涂片的溶液。该浓度与血浆等渗,可稳定粪便中脱落的白细胞和红细胞[15],因此是制备粪便涂片以进行血细胞计数的良好选择。然而,该溶液无法灭活可能污染于粪便中的SARS-CoV-2。因此,为保障实验室人员安全处理粪便样本,亟需建立一种在COVID-19疫情期间安全制备粪便涂片的新方案。

近期研究表明,多种去污剂和离液剂可完全灭活SARS-CoV-2及其他冠状病毒,如4%十二烷基硫酸钠(SDS)、1%脱氧胆酸钠(SDC)、三氟乙酸(TFA)按1:4比例混合,而6M盐酸胍(GdmCl)和8M尿素仅部分灭活[16]。氯己定葡萄糖酸盐、阴离子表面活性剂及具有介观结构的碳酸钙(CAC-717)亦显示出对SARS-CoV-2的杀病毒活性[17]。甲醛是另一种可用于灭活多种病毒的化学试剂,包括甲型流感病毒、腺病毒、巨细胞病毒、甲型肝炎病毒和脊髓灰质炎病毒[18–20]。其作用机制是与病毒蛋白的氨基酸反应,作用于N端氨基及精氨酸、半胱氨酸、组氨酸和赖氨酸残基的侧链,形成可逆的羟甲基加合物和不可逆的亚甲基桥[21]。然而,甲醛对冠状病毒的灭活活性及其在粪便检查中防止冠状病毒传播的应用尚未被广泛研究。因此,本研究旨在评估甲醛对冠状病毒(以PEDV为代表)的灭活活性,并评价其在红细胞和白细胞分析中的有效性。本研究结果将为处理含有SARS-CoV-2的粪便标本提供合适的方法。此外,值得注意的是,此类意外材料可在标准生物安全二级(BSL-2)实验室环境中安全处理。

2. 材料与方法 2.1 人体伦理 本研究经玛希隆大学诗里拉吉医院医学院诗里拉吉机构审查委员会(SIRB)审查并豁免伦理审批(协议编号:499/2564),因所用样本非直接采集自患者。

2.2 微生物与细胞系 使用猪流行性腹泻病毒(PEDV)P70株作为冠状病毒代表,该病毒对人类无致病风险,可在生物安全二级(BSL-2)实验室操作;使用耐格里阿米巴(Naegleria fowleri)CDC VO 3081株作为可自由生活的寄生虫代表,易于培养。非洲绿猴肾细胞(Vero)用于PEDV的扩增。PEDV及Vero细胞系由名誉教授Wanpen Chaicumpa博士提供,来自治疗性蛋白与抗体工程研究中心。N. fowleri由美国疾病控制与预防中心(USCDC)的GS Visvesvara博士提供。

2.3 化学试剂 0.9%(w/v)氯化钠(NaCl)生理盐水(NSS)购自Thai Nakorn Patana有限公司。10%甲醛溶液由100 mL甲醛溶液(KEMAUS,泰国曼谷)与1 L无菌蒸馏水混合配制。10%(v/v)等渗甲醛通过将0.9 g NaCl溶解于10%甲醛溶液中制备。

2.4 猪流行性腹泻病毒的扩增 PEDV在非洲绿猴肾细胞(Vero)中扩增。简言之,Vero细胞在含10%热灭活胎牛血清(FBS;HyClone,GE Healthcare Bio-Sciences Austria GmbH,奥地利帕兴)、2 mM L-丙氨酰-L-谷氨酰胺二肽(Gibco,Life Technologies Corporation,美国纽约州格兰德岛)、100 U/mL青霉素(Gibco)和100 μg/mL链霉素(Gibco)的Dulbecco改良Eagle培养基(DMEM)(Gibco)中培养,置于37°C、5% CO₂的湿润培养箱中。收集细胞后用无菌磷酸盐缓冲盐水(PBS,pH 7.4)洗涤两次,以MOI 0.001接种PEDV,继续在37°C、5% CO₂条件下培养至使用。

2.5 耐格里阿米巴的培养 N. fowleri在含10% FBS的Nelson培养基中,于T 25 cm²培养瓶(Corning,美国纽约州纽约)中37°C安全设施内培养。

2.6 冠状病毒体外灭活与噬斑形成试验 为测试10%甲醛或10%等渗甲醛是否能灭活冠状病毒,以PEDV P70株为代表进行噬斑形成试验[22]。简言之,将100 μL 10%甲醛或10%等渗甲醛与100 μL PEDV悬液(178,000 pfu)混合,室温孵育5分钟。用DMEM按1:10,000稀释后,取1 mL各混合物分别加入含Vero细胞单层的24孔组织培养板孔中(设复孔),于37°C、5% CO₂湿润培养箱中孵育1小时以允许病毒吸附。以仅含病毒的培养基作为阴性灭活对照,未感染的Vero细胞(mock)作为阴性噬斑形成对照。去除游离PEDV颗粒,用PBS洗涤细胞两次。每孔加入羧甲基纤维素(CMC)(含2 μg/mL TPCK处理胰酶的2% CMC/DMEM),继续于37°C、5% CO₂条件下孵育48小时。细胞用10%甲醛室温固定1小时,再用含10%乙醇的1%结晶紫染色。通过Vero细胞中是否形成噬斑判断PEDV是否被灭活。在40倍光学显微镜下计数噬斑数。

2.7 寄生虫灭活试验 为评估10%甲醛和10%等渗甲醛对寄生虫的灭活活性,选择N. fowleri(一种自由生活的阿米巴原虫)作为代表。将处于对数生长期的N. fowleri滋养体(1×10⁴个细胞)100 μL接种于含10% FBS、100 U/mL青霉素和100 μg/mL链霉素的Nelson培养基中,置于96孔组织培养板各孔内,37°C孵育24小时。弃去培养液后,向含阿米巴的孔中加入100 μL浓度为10%、5%和2.5%的甲醛或等渗甲醛。仅含培养基的阿米巴孔作为阴性灭活对照,含0.9% NSS的阿米巴孔作为阳性灭活对照。将平板置于37°C孵育5分钟。使用CellTiter-Glo® 3D细胞活力检测试剂盒(Promega,Promega Corporation,美国威斯康星州麦迪逊)测定各处理组中活阿米巴数量。滋养体存活率计算公式为:(测试样本发光强度 / 阴性灭活对照样本发光强度)× 100%。结果以三次独立实验的平均值±标准差(SD)表示。

2.8 粪便涂片制备 使用三种试剂制备粪便涂片:0.9% NSS(标准溶液)、10%甲醛和10%等渗甲醛(本研究开发)[23]。简言之,将一滴粪便样本与一滴0.9% NSS、10%甲醛或10%等渗甲醛在载玻片上充分混合,涂成薄层,盖上盖玻片,分别在室温下静置5、10、20和30分钟。所有实验均在玛希隆大学诗里拉吉医院医学院寄生虫学系BSL-2实验室的II级生物安全柜内进行。

2.9 寄生虫检查 在400倍显微镜下观察用0.9% NSS、10%甲醛和10%等渗甲醛制备的粪便涂片中的虫卵和寄生虫。

2.10 红细胞与白细胞计数 在400倍显微镜下计数上述各粪便涂片中的红细胞(RBC)和白细胞(WBC)数量,并按每高倍干视野(Cells/HD)分为0–1、2–3、4–5、6–10、11–20、21–30、31–50和>50个细胞范围。计数由三名独立实验技术人员完成。以百分比形式展示各涂片中检出的RBC和WBC数量。比较两种方法(0.9% NSS与10%等渗甲醛制备的涂片)的结果。

2.11 统计分析 使用IBM SPSS Statistics for Windows 21版(IBM Corp., Armonk, NY, USA)评估两种方法(10%等渗甲醛与0.9% NSS制备的粪便涂片)之间的一致性以及三名技术人员间的评分者间信度,分别以Kappa系数和Fleiss Kappa值(95%置信区间,CI)表示。p值<0.05认为差异具有统计学意义。

3. 结果与讨论 3.1 甲醛对冠状病毒的灭活活性 为测试甲醛对冠状病毒(以PEDV为代表)的灭活活性,将PEDV在室温下用10%甲醛或10%等渗甲醛处理5分钟。以Vero细胞为宿主,通过噬斑形成试验评估病毒活力(图1a)。结果显示,10%甲醛和10%等渗甲醛处理5分钟后可完全灭活PEDV。经10%甲醛或10%等渗甲醛处理的PEDV未形成噬斑,而未处理的PEDV则可见噬斑(图1b)。该数据表明,PEDV作为冠状病毒的一种,可在短时间内(5分钟)被甲醛中和。此前已有报道显示,PEDV对4%无水碳酸钠、1%磷酸碘伏和2%氢氧化钠敏感[24]。尽管已有研究报道1%甲醛可灭活PEDV[24],但其等渗形式尚未被研究。本研究首次报道了等渗甲醛对PEDV的灭活活性。在作用持续时间方面,本研究结果与先前研究一致:SARS-CoV-2可被Trizol和Trizol LS(病毒:Trizol试剂=1:4)在室温下5分钟内完全灭活[25]。同时,0.5% SDS、0.5% Triton X-100、0.5% NP-40、100%甲醇和4%多聚甲醛也可在室温下中和SARS-CoV-2,但需更长时间(30分钟)[25]。由于PEDV与SARS-CoV-2同属冠状病毒科,共享相似的生化与生物学特性(如膜融合过程、M蛋白整体折叠等)[2,26],两者对甲醛的敏感性可能相同。因此,10%甲醛和10%等渗甲醛是处理含SARS-CoV-2样本的实验室中理想的病毒灭活剂。

图1. 10%甲醛和10%等渗甲醛对猪流行性腹泻病毒(PEDV)的灭活活性:(a)体外灭活试验流程图。(b)室温处理5分钟后,经10%甲醛和10%等渗甲醛处理的PEDV每孔噬斑数。以仅含病毒的培养基作为阴性灭活对照,未感染的Vero细胞(mock)作为阴性噬斑形成对照。结果以三次独立实验的平均值±标准差(SD)表示。

3.2 甲醛对自由生活寄生虫的灭活作用 为测试甲醛对寄生虫的灭活能力,选择N. fowleri(一种通过污染水源或灰尘经鼻腔侵入人体、引起原发性阿米巴脑膜脑炎的自由生活阿米巴[27])作为代表,在不同浓度下进行甲醛和等渗甲醛的体外抑制试验。使用CellTiter-Glo® 3D细胞活力检测试剂盒(基于ATP定量准确测定细胞活力[28])评估寄生虫活力(图2a)。结果显示,所有浓度(10%、5%和2.5%)的甲醛和等渗甲醛在37°C下处理5分钟均可完全灭活寄生虫,而未处理的寄生虫仍存活(图2b)。该结果与先前研究一致:10%甲醛在室温下可杀死弓形虫卵囊,但需4天处理时间[29];0.1%甲醛亦可杀死利什曼原虫前鞭毛体,但需过夜处理[30]。正如预期,0.9% NSS亦能抑制N. fowleri生长,因该生物为广盐性耐受生物。已有报道指出,Naegleria spp.在0.2% NaCl条件下生长受抑制[31]。本研究发现,尽管N. fowleri被完全灭活,其形态仍保持完整(数据未显示)。为验证此结果,随后采集粪便样本,分别用10%甲醛和10%等渗甲醛制备涂片,并与标准方法制备的涂片比较虫卵和寄生虫的检出情况。结果显示,在0.9% NSS制备的涂片中观察到的Blastocystis spp.空泡型,在10%甲醛和10%等渗甲醛制备的涂片中亦可见;但在0.9% NSS和10%等渗甲醛制备的涂片中,其空泡结构更为清晰(图3)。因此可得出结论:除冠状病毒外,甲醛对寄生虫亦具有灭活活性,且能保留寄生虫形态,有利于粪便检查。甲醛能维持寄生虫结构并不意外,因其是常用于新鲜样本(包括粪便样本)的固定剂,通过渗透样本、结合所有蛋白质中的氨基酸、与未带电的反应性氨基基团反应并形成交联结构来稳定生物结构[32]。但需注意,对于依赖运动性进行诊断的寄生虫,甲醛不适用。

图2. 不同浓度甲醛和等渗甲醛对Naegleria fowleri的灭活活性:(a)灭活试验流程图。(b)37°C处理5分钟后,经甲醛和等渗甲醛处理的N. fowleri滋养体存活率。结果以三次独立实验的平均值±标准差(SD)表示。

图3. 粪便涂片中寄生虫的存在。使用不同溶液制备粪便涂片:0.9%生理盐水(NSS)(左)、10%甲醛(中)、10%等渗甲醛(右)。可见虫卵和寄生虫。比例尺每格代表0.25微米。红色箭头指示Blastocystis spp.的空泡型。各图右下角显示空泡型的放大图像。

3.3 使用甲醛制备粪便涂片进行红细胞和白细胞分析 除检查虫卵和寄生虫外,寄生虫学实验室还需计数粪便样本中的红细胞和白细胞,以评估其他胃肠道感染。鉴于10%甲醛和10%等渗甲醛对冠状病毒和寄生虫均具有灭活活性,若其亦可用于制备粪便涂片以进行RBC和WBC计数,将具有重要价值。为此,应用10%甲醛和10%等渗甲醛制备粪便涂片,并测试其对RBC和WBC的稳定效果(图4a)。结果显示,10%甲醛无法维持粪便样本中的红细胞(图4b);使用10%甲醛制备涂片时可见红细胞溶解。相反,10%等渗甲醛或0.9% NSS(标准溶液)制备的粪便涂片在制备后0和30分钟均可稳定RBC和WBC(图4b)。该证据支持使用10%等渗甲醛制备粪便涂片,因其既能稳定红细胞和白细胞,又具有灭活冠状病毒的活性。

图4. 10%甲醛和10%等渗甲醛在0和30分钟对血细胞的稳定作用:(a)粪便涂片制备与血细胞分析流程图。(b)与标准溶液0.9%生理盐水(NSS)相比,10%甲醛和10%等渗甲醛制备的粪便涂片中红、白细胞的持久性。比例尺每格代表0.25微米。红色箭头指示红细胞(RBC),绿色箭头指示白细胞(WBC)。各图右上角和左上角分别显示白细胞和红细胞的放大图像。

为验证10%等渗甲醛用于粪便涂片法定量评估RBC和WBC的能力,选取59份经标准方法(0.9% NSS制备涂片)检出RBC或WBC的粪便样本,用10%等渗甲醛重新制备涂片。结果显示,所有经10%等渗甲醛制备的涂片中亦检出RBC和WBC。多数粪便涂片(27.1%和25.4%)中RBC和WBC数量超过50个/高倍干视野(cells/HD)(表1)。

表1. 使用10%等渗甲醛制备的粪便涂片中检出不同数量(Cells/HD)RBC和WBC的样本数(百分比)(n = 59)。

| 血细胞数量 (Cells/HD¹) | 红细胞 数量(%) | 白细胞 数量(%) | |------------------------|----------------|----------------| | 0–1 | 7 (11.9) | 12 (20.3) | | 2–3 | 10 (16.9) | 11 (18.6) | | 4–5 | 7 (11.9) | 9 (15.3) | | 6–10 | 5 (8.5) | 6 (10.2) | | 11–20 | 2 (3.4) | 4 (6.8) | | 21–30 | 11 (18.6) | 2 (3.4) | | 31–50 | 1 (1.7) | ND² | | >50 | 16 (27.1) | 15 (25.4) | | 总计 | 59 (100.0) | 59 (100.0) |

¹ 高倍干视野。² 未检出。

此外,10%等渗甲醛制备的粪便涂片中血细胞数量与0.9% NSS制备的涂片在所有定义细胞范围和时间间隔内均高度一致(Kappa系数为1.00)(表2)。两种方法在所有时间间隔的解释结果一致性亦高达100%(表2)。这些数据表明,10%等渗甲醛是粪便涂片中血细胞的有效稳定剂。

表2. 不同时间间隔下,10%等渗甲醛与标准方法(0.9% NSS制备粪便涂片)检测RBC和WBC的一致性测量(n = 59)。

| 时间(分钟) | Kappa系数值 | 可靠数据一致性 | p值 | |--------------|-------------|----------------|---------| | 5 | 1.00 | 59 (100%) | <0.001¹ | | 10 | 1.00 | 59 (100%) | <0.001¹ | | 20 | 1.00 | 59 (100%) | <0.001¹ | | 30 | 1.00 | 59 (100%) | <0.001¹ |

¹ p值<0.05,差异具有统计学意义。

为评估技术人员间血细胞计数的一致性信度,三名技术人员独立对10%等渗甲醛或0.9% NSS制备的粪便涂片进行RBC和WBC计数(图3a)。结果显示,阳性血细胞样本数量无差异(RBC和WBC的Fleiss Kappa值分别为0.918和0.932)(表3)。

表3. 三名独立技术人员间血细胞计数的一致性信度(评分者间信度)。

| 血细胞类型 | Fleiss Kappa值(95% CI) | p值 | |------------|--------------------------|---------| | RBC | 0.918 (0.852–0.983) | <0.001¹ | | WBC | 0.932 (0.865–0.998) | <0.001¹ |

¹ p值<0.05,差异具有统计学意义。

本研究证实,10%等渗甲醛可在体外完全灭活猪流行性腹泻病毒,且由于SARS-CoV-2与其他冠状病毒具有相似的生化与生物学特性,该试剂很可能对所有冠状病毒(尤其是SARS-CoV-2)均有效。此外,10%等渗甲醛亦能灭活寄生虫代表N. fowleri,且不破坏其结构;同时还能保存红细胞和白细胞,表明其可用于其他病原体感染的RBC和WBC分析。上述证据可为处理可能含有SARS-CoV-2生物标本的所有临床和科研实验室提供安全操作指导。尽管甲醛仍存在危害,但通过使用口罩和专用通风系统可显著降低风险[33]。

4. 结论 在COVID-19疫情期间,为诊断寄生虫感染及检测RBC和WBC以调查其他胃肠道感染,可使用10%等渗甲醛替代0.9% NSS制备粪便涂片,以确保常规粪便检查下游处理的安全性。该试剂不仅能灭活冠状病毒和寄生虫,还能稳定粪便涂片中的红细胞和白细胞。因此,10%等渗甲醛可用于制备粪便涂片,保障实验室人员在COVID-19疫情期间的安全操作。

作者贡献:概念化,A.T., P.C., P.R.;方法学,A.T., P.C., P.R.;形式分析,P.C., P.R.;调查,N.S., P.C., S.W., T.T., W.B.;资源,P.C., P.R.;数据整理,P.C., P.R.;撰写初稿,P.C.;审阅与编辑,A.T., P.R.;可视化,P.C., P.R., T.T., W.B.;监督,A.T., P.R.;项目管理,P.C.;经费获取,P.C.。所有作者均已阅读并同意稿件发表。

资助:本研究由玛希隆大学诗里拉吉医院医学院诗里拉吉研究发展基金(由“常规转研究”项目R2R管理)资助,项目编号R016435049。A.T.和P.R.为玛希隆大学诗里拉吉医院医学院“Chalermphrakiat”资助学者。

机构审查委员会声明:本研究伦理审查与批准已被豁免,因所有粪便标本均采集自实验室库存。

知情同意声明:不适用。

数据可用性声明:不适用。

致谢:作者衷心感谢泰国曼谷玛希隆大学诗里拉吉医院医学院临床研究部临床流行病学分部Nerisa Thornsri在统计分析方面的支持。特别感谢玛希隆大学诗里拉吉医院医学院研究部“常规转研究”单元副