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Article(id=1217845639136858618, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250415002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1744646400000, receivedDateStr=2025-04-15, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768286626848, onlineDateStr=2026-01-13, pubDate=1756051200000, pubDateStr=2025-08-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768286626848, onlineIssueDateStr=2026-01-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768286626848, creator=13701087609, updateTime=1768286626848, updator=13701087609, issue=Issue{id=1217845635080962613, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='16', pageStart='1', pageEnd='324', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1768286625881, creator=13701087609, updateTime=1768287480278, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217849218753024879, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217849218753024880, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=247, endPage=253, ext={EN=ArticleExt(id=1217845639568871949, articleId=1217845639136858618, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Etiological study of a food poisoning incident caused by venison, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To analyze the cause of a complex food poisoning incident using a combination of non-targeted and targeted methods based on mass spectrometry. Methods Suspected contaminated food and blood samples from the cases were collected. After sample preparation, a high-resolution mass spectrometry non-targeted method was used for toxin screening, and a triple quadrupole mass spectrometry targeted detection method was applied for the quantitative analysis of xylazine in the samples. Results Xylazine was detected in both the suspected contaminated food (raw and fried venison) and the serum samples of 3 cases. The concentrations in raw and fried venison were 3.0 μg/kg and 395.9 μg/kg, while the concentrations in the cases’ serum were 47.0, 16.0 and 15.6 ng/mL, respectively. Conclusion This incident is confirmed as xylazine poisoning caused by venison ingestion. First, through epidemiological investigation, the scope for identifying the cause of poisoning can be quickly determined. The non-targeted method provides accurate evidence for clinical treatment, aiding in the diagnosis and management of such events. At the same time, the targeted quantitative analysis of samples also provides a basis for the formulation of drug use standards in farmed animals in the future.

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目的 通过流行病学调查、质谱仪器方法联合, 对一起由食用鹿肉引起的疑难食物中毒事件进行病因学研究。方法 采集疑似中毒食物和病例血液样本, 先采用高分辨质谱非靶向方法进行毒因筛查与确证, 再通过三重四极杆质谱靶向检测方法对样本中赛拉嗪含量进行定量分析。结果 疑似中毒食物(生鹿肉和炒鹿肉)以及3位病例的血清样本均检出赛拉嗪, 在生鹿肉与炒鹿肉中含量分别为3.0 μg/kg、395.9 μg/kg, 病例血清中赛拉嗪的含量分别为47.0、16.0、15.6 ng/mL。结论 本起事件确定为食用鹿肉导致的赛拉嗪中毒事件, 先通过流行病学调查快速圈定中毒病因的鉴定范围, 非靶向筛查方法为中毒病因快速鉴定确定提供了技术支持, 为中毒事件的快速处置和临床精准救治提供了依据, 同时对中毒样本进行靶向定量分析也为动物养殖用药标准的制定提供依据。

, correspAuthors=马浩嘉, authorNote=null, correspAuthorsNote=
* 马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:
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马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:

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马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:

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马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:

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Detection of two food poisoning cases caused by xylazine residual using liquid chromatography-mass spectrometry[J]. Chinese Journal of Health Laboratory Technology, 2023, 33(13): 1540-1544., articleTitle=Detection of two food poisoning cases caused by xylazine residual using liquid chromatography-mass spectrometry, refAbstract=null), Reference(id=1217864276312768663, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2016, volume=33, issue=8, pageStart=569, pageEnd=null, url=null, language=null, rfNumber=[26], rfOrder=35, authorNames=于松松, 张一杰, 王真, journalName=临床内科杂志, refType=null, unstructuredReference=于松松, 张一杰, 王真. 赛拉嗪中毒两例[J]. 临床内科杂志, 2016, 33(8): 569., articleTitle=赛拉嗪中毒两例, refAbstract=null), Reference(id=1217864276463763617, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2016, volume=33, issue=8, pageStart=569, pageEnd=null, url=null, language=null, rfNumber=[26], rfOrder=36, authorNames=YU SS, ZHANG YJ, WANG Z, journalName=Journal of Clinical Internal Medicine, refType=null, unstructuredReference=YU SS, ZHANG YJ, WANG Z. Two cases of cetirizine intoxication[J]. Journal of Clinical Internal Medicine, 2016, 33(8): 569., articleTitle=Two cases of cetirizine intoxication, refAbstract=null), Reference(id=1217864276551844005, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2022, volume=60, issue=8, pageStart=892, pageEnd=901, url=null, language=null, rfNumber=[27], rfOrder=37, authorNames=BALL NS, KNABLE BM, RELICH TA, journalName=Clinical Toxicology, refType=null, unstructuredReference=BALL NS, KNABLE BM, RELICH TA, et al. Xylazine poisoning: A systematic review[J]. Clinical Toxicology, 2022, 60(8): 892-901., articleTitle=Xylazine poisoning: A systematic review, refAbstract=null), Reference(id=1217864276635730088, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2011, volume=124, issue=13, pageStart=2068, pageEnd=2070, url=null, language=null, rfNumber=[28], rfOrder=38, authorNames=ZHANG L, FANG ZJ, LIU F, journalName=Chinese Medical Journal (English), refType=null, unstructuredReference=ZHANG L, FANG ZJ, LIU F, et al. Magnetic resonance imaging and magnetic resonance angiography in severe crush syndrome with consideration of fasciotomy or amputation: A novel diagnostic tool[J]. Chinese Medical Journal (English), 2011, 124(13): 2068-2070., articleTitle=Magnetic resonance imaging and magnetic resonance angiography in severe crush syndrome with consideration of fasciotomy or amputation: A novel diagnostic tool, refAbstract=null), Reference(id=1217864276728004780, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2019, volume=298, issue=null, pageStart=307, pageEnd=311, url=null, language=null, rfNumber=[29], rfOrder=39, authorNames=CAMPOBASSO CP, DE-MICCO F, BUGELLI V, journalName=Forensic Science International, refType=null, unstructuredReference=CAMPOBASSO CP, DE-MICCO F, BUGELLI V, et al. Undetected traumatic diastasis of cranial sutures: A case of child abuse[J]. Forensic Science International, 2019, 298: 307-311, articleTitle=Undetected traumatic diastasis of cranial sutures: A case of child abuse, refAbstract=null), Reference(id=1217864276824473776, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, doi=null, pmid=null, pmcid=null, year=2024, volume=7, issue=1, pageStart=e2350630, pageEnd=null, url=null, language=null, rfNumber=[30], rfOrder=40, authorNames=CANO M, DANIULAITYTE R, MARSIGLIA F, journalName=JAMA Network Open, refType=null, unstructuredReference=CANO M, DANIULAITYTE R, MARSIGLIA F. Xylazine in overdose deaths and forensic drug reports in US States, 2019—2022[J]. JAMA Network Open, 2024, 7(1): e2350630., articleTitle=Xylazine in overdose deaths and forensic drug reports in US States, 2019—2022, refAbstract=null)], funds=[Fund(id=1217864270570767197, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, awardId=SZXK066, language=CN, fundingSource=深圳市医学重点学科建设经费资助项目(SZXK066), fundOrder=null, country=null), Fund(id=1217864270667236197, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, awardId=24959, language=CN, fundingSource=国际原子能机构项目(24959), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1217864261364269400, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, xref=1, ext=[AuthorCompanyExt(id=1217864261372658009, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, companyId=1217864261364269400, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China), AuthorCompanyExt(id=1217864261376852314, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, companyId=1217864261364269400, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 深圳市疾病预防控制中心, 深圳 518055)]), AuthorCompany(id=1217864261565596016, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, xref=2, ext=[AuthorCompanyExt(id=1217864261578178930, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, companyId=1217864261565596016, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Shenzhen Guangming Center for Disease Control and Prevention, Shenzhen 518106, China), AuthorCompanyExt(id=1217864261603344760, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, companyId=1217864261565596016, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 深圳市光明区疾病预防控制中心, 深圳 518106)])], figs=[ArticleFig(id=1217864266514875046, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Fig.1, caption=MS information of xylazine in fried venison sample, figureFileSmall=z6GXYi3/Rbc69mAtOtdpMA==, figureFileBig=9F32m12djf9+Uwu1cesEJw==, tableContent=null), ArticleFig(id=1217864266607149743, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=图1, caption=炒鹿肉样品中赛拉嗪MS信息

注: A. 赛拉嗪[M+H]+(m/z 221.11)的提取离子色谱(extracted ion chromatogram, XIC)图; B. 实测同位素分布; C. 实测二级质谱信息(蓝色)与物质库二级质谱信息(灰色), 图2~3同。

, figureFileSmall=z6GXYi3/Rbc69mAtOtdpMA==, figureFileBig=9F32m12djf9+Uwu1cesEJw==, tableContent=null), ArticleFig(id=1217864266753950394, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Fig.2, caption=MS information of xylazine in raw venison sample, figureFileSmall=j+VIaKCXwx9ekkZbUkcPmw==, figureFileBig=kFCcRm8Rr48z9K1Vp8VdfA==, tableContent=null), ArticleFig(id=1217864266875585217, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=图2, caption=生鹿肉样品中赛拉嗪MS信息, figureFileSmall=j+VIaKCXwx9ekkZbUkcPmw==, figureFileBig=kFCcRm8Rr48z9K1Vp8VdfA==, tableContent=null), ArticleFig(id=1217864266997220041, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Fig.3, caption=MS information of xylazine in blood sample of patient 1, figureFileSmall=QYGImwavGVG3qU4vQLrbbA==, figureFileBig=HU1azqu7k4i9wb0nxWE5Ag==, tableContent=null), ArticleFig(id=1217864267144020689, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=图3, caption=病人1血液样品中赛拉嗪MS信息, figureFileSmall=QYGImwavGVG3qU4vQLrbbA==, figureFileBig=HU1azqu7k4i9wb0nxWE5Ag==, tableContent=null), ArticleFig(id=1217864267278238427, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Fig.4, caption=Retention time of xylazine standard (0.5 μg/mL) (A) and xylazine in matrix sample of blank raw venison (B), figureFileSmall=Kg7e6zbzL81cndEB6zujiQ==, figureFileBig=mYN+dJEQov6ebAZFUXIOXg==, tableContent=null), ArticleFig(id=1217864267420844771, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=图4, caption=赛拉嗪标准品-0.5 μg/mL (A)与空白鹿肉基质加标样品(B)的保留时间, figureFileSmall=Kg7e6zbzL81cndEB6zujiQ==, figureFileBig=mYN+dJEQov6ebAZFUXIOXg==, tableContent=null), ArticleFig(id=1217864267567645419, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Fig.5, caption=Fragmentation pattern of xylazine, figureFileSmall=6GCa32rWqAl9AQKnGwKqOQ==, figureFileBig=xCByGeMXhUd0zpeCOxK/EQ==, tableContent=null), ArticleFig(id=1217864267710251760, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=图5, caption=赛拉嗪的裂解规律, figureFileSmall=6GCa32rWqAl9AQKnGwKqOQ==, figureFileBig=xCByGeMXhUd0zpeCOxK/EQ==, tableContent=null), ArticleFig(id=1217864267857052408, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Table 1, caption=

Parameters of MS for xylazine and its internal standard

, figureFileSmall=null, figureFileBig=null, tableContent=
物质名 Q1 (m/z) Q3 (m/z) 碰撞能量/V 去簇电压/V
赛拉嗪 221.1 164.1* 49 60
221.1 147.1 40 60
赛拉嗪-D6 227.1 90.2* 30 60
), ArticleFig(id=1217864269274727167, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=表1, caption=

赛拉嗪及其内标的MS采集参数

, figureFileSmall=null, figureFileBig=null, tableContent=
物质名 Q1 (m/z) Q3 (m/z) 碰撞能量/V 去簇电压/V
赛拉嗪 221.1 164.1* 49 60
221.1 147.1 40 60
赛拉嗪-D6 227.1 90.2* 30 60
), ArticleFig(id=1217864269408944900, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Table 2, caption=

Complete blood count, coagulation assays and biochemical tests of patients

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 指标 血中指标水平
病人1 病人2 病人3
1 红细胞计数/L 4.17×1012↑ - -
2 红细胞比积/% 38.4↓ - -
3 白细胞计数/L - - 10.86×109↑
4 淋巴细胞绝对值/L - - 0.77×109↓
5 淋巴细胞百分率/% 16.00↓ - 7.10↑
6 单核细胞百分率/% 10.10↑ - 2.90↓
7 中性粒细胞绝对值/L 6.88×109↑ - 9.73×109↑
8 中性粒细胞百分率/% - - 89.60↑
9 嗜酸性细胞百分率/% - 0.30↓ 0.20↓
10 单核细胞绝对值/L 0.95×109↑ 0.70×109↑ -
11 血小板体积分布宽度/fL - - 8.60↓
12 血小板平均体积分布宽度/fL - - 8.70↓
13 纤维蛋白原/(g/L) 3.79↑ - -
14 钾/(mmol/L) 3.45↓ - -
15 钠/(mmol/L) 135.7↓ 133.3↓ 133.3↓
16 白蛋白/(g/L) 38.9↓ 39.5↓ -
17 总蛋白/(g/L) - 64.7↓ -
18 尿素/(mmol/L) 8.38↑ - -
19 尿酸/(mmol/L) 593.2↑ - -
20 胆碱酯酶/(U/L) 5811.4↓ - -
), ArticleFig(id=1217864269534774031, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=表2, caption=

病人血常规、急凝血与血生化指标检测结果

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 指标 血中指标水平
病人1 病人2 病人3
1 红细胞计数/L 4.17×1012↑ - -
2 红细胞比积/% 38.4↓ - -
3 白细胞计数/L - - 10.86×109↑
4 淋巴细胞绝对值/L - - 0.77×109↓
5 淋巴细胞百分率/% 16.00↓ - 7.10↑
6 单核细胞百分率/% 10.10↑ - 2.90↓
7 中性粒细胞绝对值/L 6.88×109↑ - 9.73×109↑
8 中性粒细胞百分率/% - - 89.60↑
9 嗜酸性细胞百分率/% - 0.30↓ 0.20↓
10 单核细胞绝对值/L 0.95×109↑ 0.70×109↑ -
11 血小板体积分布宽度/fL - - 8.60↓
12 血小板平均体积分布宽度/fL - - 8.70↓
13 纤维蛋白原/(g/L) 3.79↑ - -
14 钾/(mmol/L) 3.45↓ - -
15 钠/(mmol/L) 135.7↓ 133.3↓ 133.3↓
16 白蛋白/(g/L) 38.9↓ 39.5↓ -
17 总蛋白/(g/L) - 64.7↓ -
18 尿素/(mmol/L) 8.38↑ - -
19 尿酸/(mmol/L) 593.2↑ - -
20 胆碱酯酶/(U/L) 5811.4↓ - -
), ArticleFig(id=1217864269652214553, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Table 3, caption=

Non-targeted screening results of toxic samples

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 样品 检出
毒物		 理论值
(m/z)		 实测值
(m/z)		 误差
/ppm
1 酸菜炒鹿肉 赛拉嗪 221.111 221.1099 -3.4
2 生鹿肉 赛拉嗪 221.111 221.1103 -1.7
3 病人1血液 赛拉嗪 221.111 221.1104 -1.1
4 病人2血液 赛拉嗪 221.111 221.1108 0.4
5 病人3血液 赛拉嗪 221.111 221.1106 -0.5
), ArticleFig(id=1217864269832569637, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=表3, caption=

中毒样本非靶向筛查结果

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 样品 检出
毒物		 理论值
(m/z)		 实测值
(m/z)		 误差
/ppm
1 酸菜炒鹿肉 赛拉嗪 221.111 221.1099 -3.4
2 生鹿肉 赛拉嗪 221.111 221.1103 -1.7
3 病人1血液 赛拉嗪 221.111 221.1104 -1.1
4 病人2血液 赛拉嗪 221.111 221.1108 0.4
5 病人3血液 赛拉嗪 221.111 221.1106 -0.5
), ArticleFig(id=1217864269950010157, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Table 4, caption=

Secondary ion scanning results and fragment structure analysis of xylazine standard

, figureFileSmall=null, figureFileBig=null, tableContent=
一级离子 二级离子
理论值(m/z) 实测值(m/z) 误差/ppm 理论值(m/z) 实测值(m/z) 误差/ppm 预测分子式 丰度/%
221.111 221.1114 3.3 164.0528 164.0522 -3.9 C9H10NS+ 100.00
147.0917 147.0918 0.9 C9H11N2+ 38.46
130.0651 130.0656 3.3 C6H12NS+ 35.06
121.0886 121.0890 2.9 C8H11N+ 26.17
120.0808 120.0811 2.3 C8H10N+ 38.42
105.0699 105.0698 -1.0 C8H9+ 23.14
90.0372 90.0370 2.4 C3H8NS+ 79.25
), ArticleFig(id=1217864270075839286, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=表4, caption=

赛拉嗪标准品二级离子扫描结果与碎片结构分析

, figureFileSmall=null, figureFileBig=null, tableContent=
一级离子 二级离子
理论值(m/z) 实测值(m/z) 误差/ppm 理论值(m/z) 实测值(m/z) 误差/ppm 预测分子式 丰度/%
221.111 221.1114 3.3 164.0528 164.0522 -3.9 C9H10NS+ 100.00
147.0917 147.0918 0.9 C9H11N2+ 38.46
130.0651 130.0656 3.3 C6H12NS+ 35.06
121.0886 121.0890 2.9 C8H11N+ 26.17
120.0808 120.0811 2.3 C8H10N+ 38.42
105.0699 105.0698 -1.0 C8H9+ 23.14
90.0372 90.0370 2.4 C3H8NS+ 79.25
), ArticleFig(id=1217864270222639939, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=EN, label=Table 5, caption=

Working curves, precisions and average recovery rates of quantitative method

, figureFileSmall=null, figureFileBig=null, tableContent=
样品种类 工作曲线 相关系数(r) 添加浓度 精密度/% 平均回收率/%
空白生鹿肉 Y=21.00455X+54.31402 0.9993 10 μg/kg 3.2 94.2
20 μg/kg 0.9 128.2
100 μg/kg 3.2 122.3
空白血清 Y=0.00759X+0.00284 0.9998 1 ng/mL 5.9 118.8
2 ng/mL 1.5 108.0
10 ng/mL 1.8 99.3
), ArticleFig(id=1217864270327497548, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845639136858618, language=CN, label=表5, caption=

定量方法的工作曲线、精密度和平均回收率

, figureFileSmall=null, figureFileBig=null, tableContent=
样品种类 工作曲线 相关系数(r) 添加浓度 精密度/% 平均回收率/%
空白生鹿肉 Y=21.00455X+54.31402 0.9993 10 μg/kg 3.2 94.2
20 μg/kg 0.9 128.2
100 μg/kg 3.2 122.3
空白血清 Y=0.00759X+0.00284 0.9998 1 ng/mL 5.9 118.8
2 ng/mL 1.5 108.0
10 ng/mL 1.8 99.3
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一起鹿肉引起食物中毒事件的病因学研究
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马浩嘉 1, * , 许欣欣 1 , 朱舟 1 , 刘红河 1 , 陈映新 2
食品安全质量检测学报 | 食品分析与检测 2025,16(16): 247-253
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食品安全质量检测学报 | 食品分析与检测 2025, 16(16): 247-253
一起鹿肉引起食物中毒事件的病因学研究
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马浩嘉1, * , 许欣欣1, 朱舟1, 刘红河1, 陈映新2
作者信息
  • 1 深圳市疾病预防控制中心, 深圳 518055
  • 2 深圳市光明区疾病预防控制中心, 深圳 518106

    • 马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:

通讯作者:

* 马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:
Etiological study of a food poisoning incident caused by venison
Hao-Jia MA1, * , Xin-Xin XU1, Zhou ZHU1, Hong-He LIU1, Ying-Xin CHEN2
Affiliations
  • 1 Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China
  • 2 Shenzhen Guangming Center for Disease Control and Prevention, Shenzhen 518106, China
出版时间: 2025-08-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250415002
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摘要
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目的 通过流行病学调查、质谱仪器方法联合, 对一起由食用鹿肉引起的疑难食物中毒事件进行病因学研究。方法 采集疑似中毒食物和病例血液样本, 先采用高分辨质谱非靶向方法进行毒因筛查与确证, 再通过三重四极杆质谱靶向检测方法对样本中赛拉嗪含量进行定量分析。结果 疑似中毒食物(生鹿肉和炒鹿肉)以及3位病例的血清样本均检出赛拉嗪, 在生鹿肉与炒鹿肉中含量分别为3.0 μg/kg、395.9 μg/kg, 病例血清中赛拉嗪的含量分别为47.0、16.0、15.6 ng/mL。结论 本起事件确定为食用鹿肉导致的赛拉嗪中毒事件, 先通过流行病学调查快速圈定中毒病因的鉴定范围, 非靶向筛查方法为中毒病因快速鉴定确定提供了技术支持, 为中毒事件的快速处置和临床精准救治提供了依据, 同时对中毒样本进行靶向定量分析也为动物养殖用药标准的制定提供依据。

食物中毒  /  赛拉嗪  /  非靶向筛查  /  流行病学调查

Objective To analyze the cause of a complex food poisoning incident using a combination of non-targeted and targeted methods based on mass spectrometry. Methods Suspected contaminated food and blood samples from the cases were collected. After sample preparation, a high-resolution mass spectrometry non-targeted method was used for toxin screening, and a triple quadrupole mass spectrometry targeted detection method was applied for the quantitative analysis of xylazine in the samples. Results Xylazine was detected in both the suspected contaminated food (raw and fried venison) and the serum samples of 3 cases. The concentrations in raw and fried venison were 3.0 μg/kg and 395.9 μg/kg, while the concentrations in the cases’ serum were 47.0, 16.0 and 15.6 ng/mL, respectively. Conclusion This incident is confirmed as xylazine poisoning caused by venison ingestion. First, through epidemiological investigation, the scope for identifying the cause of poisoning can be quickly determined. The non-targeted method provides accurate evidence for clinical treatment, aiding in the diagnosis and management of such events. At the same time, the targeted quantitative analysis of samples also provides a basis for the formulation of drug use standards in farmed animals in the future.

food poisoning  /  xylazine  /  non-targeted screening  /  epidemiological investigation
马浩嘉, 许欣欣, 朱舟, 刘红河, 陈映新. 一起鹿肉引起食物中毒事件的病因学研究. 食品安全质量检测学报, 2025 , 16 (16) : 247 -253 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250415002
Hao-Jia MA, Xin-Xin XU, Zhou ZHU, Hong-He LIU, Ying-Xin CHEN. Etiological study of a food poisoning incident caused by venison[J]. Journal of Food Safety & Quality, 2025 , 16 (16) : 247 -253 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250415002
正文
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0 引言
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食物中毒是全世界最常见的疾病之一[1]。在中国, 随着居民对食品生产、储存等安全意识提升[2-3], 如何防范与处理细菌性和化学性食物中毒已成为广受关注的热点。细菌性食物中毒的发生率高、波及面广, 根据食源性疾病监测系统的报告, 中国2011年至2022年间报道413起致泻性大肠杆菌引起的食物中毒事件, 共有8127人患病, 2565人住院, 1人死亡[4]; 而化学性食物中毒危害性也不容忽视, 仅浙江省2011年到2023年间报道的74起化学性食物中毒事件便导致461人患病, 209人住院, 1人死亡[5]。考虑到食物中毒普遍存在漏报情况(部分发展中国家漏报率高达95%), 食物中毒情况实际可能比报道更为严重[6]。除发生率高、危害性强的特点外, 食物中毒的成因多样且复杂[7], 各类毒物如生物碱[8-9]、河豚毒素[10]、蘑菇毒素[11]、兽药[12]、鼠药[13-14]、农药[15]引发的多例食物中毒事件报道层出不穷, 因此如何精准判定起因与及时救治便成为亟待解决的重要问题。目前依靠流行病学调查和临床诊断可以通过毒素的分布、产生规律以及毒理学研究对常见毒素进行推测与分析, 但对于不常见的毒素以及化学物质, 由于其种类繁多且应用场景广泛, 流行病学调查和临床诊断往往无法进行准确判定。
质谱检测法是筛查鉴定食物中有毒化学物质的新兴手段, 其中以高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/ MS)[16-18]或气相色谱-串联质谱法[19-20]中的靶向检测方法最为常见。这些仪器的分辨率不足以区分质荷比(mass-to-charge ratio, m/z)相似的干扰物质, 也需要对应标准品对假阳性结果进行排除。以高效液相色谱-串联四极杆飞行时间质谱为代表的高分辨质谱的非靶向检测方法则能支持在毒素种类繁多、缺乏标准物质的情况的精准筛查工作, 准确鉴定毒因[21], 但由于使用成本高、人员专业性要求等问题并未被广泛应用。
本研究基于深圳市发生的一起疑难食物中毒事件, 通过联合流行病学调查、高分辨质谱非靶向方法和HPLC-MS/MS靶向方法, 综合分析其中毒成因与毒物浓度, 赛拉嗪病例为中毒事件的快速处置、临床精准救治和动物养殖用药标准的制定提供有力依据。
1 材料与方法
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1.1 材料、仪器与试剂
空白样品包括空白血液(经合法的公共卫生实践后的剩余样本)和空白鹿肉(网购获取); 1.5 mL离心管(美国Axygen公司); 50 mL离心管(美国Corning公司); 针式过滤器(0.22 μm, 中国安谱公司)。
QTOF X500R高效液相色谱串联四极杆飞行时间质谱仪、QTRAP 6500高效液相串联三重四极杆质谱仪(美国AB SCIEX公司); Luna Omega C18色谱柱(100 mm×2.1 mm, 1.6 μm, 美国Phenomenex公司); IQ 7000超纯水系统(美国Milli-Q公司); MS3型漩涡振荡器(德国IKA公司); Microfuge 20 Centrifuge高转速低温离心机、Avanti J-26 XP Centrifuge立式高速冷冻离心机(美国Beckman Coulter公司); E300 H超声振荡器(德国Elmasonic公司); SCI506桌面血清离心机(美国Scilogex公司); TurboVap氮气浓缩仪(瑞典Biotage公司); GM 200研磨匀浆器(德国Retsch公司)。
甲醇、乙腈、正己烷(色谱纯)、甲酸(纯度98%~100%)、甲酸铵(纯度≥99%)(徳国Merck公司); 赛拉嗪标准品(纯度>99%)(CAS: 7361-61-7)、对应内标赛拉嗪-D6(纯度>99%)(CAS: 1228182-53-3)(天津阿尔塔科技有限公司); 实验用水由超纯水系统处理后所得。
1.2 方法
1.2.1 流行病学调查
采用描述性流行病学调查方法对中毒事件进行现场调查, 在就餐点进行食谱调查并采集食用残余食物, 采集到病例烹饪残余生鹿肉约20 g及吃剩的炒鹿肉约30 g, 共2份样品。本次中毒病例共3名, 通过面对面访谈, 追溯病例发病前饮食情况和事件经过, 并通过接诊医生收集病例入院的首次采集血液样品(每位病例约4 mL)、临床症状、诊断、检查和治疗用药等信息。
1.2.2 样品的前处理
血液样品经3800 r/min离心5 min, 转移上层血清备用。生鹿肉与炒鹿肉均使用匀浆器充分粉碎并搅拌均匀后备用。
血清: 取100 μL血清于1.5 mL离心管中, 加入200 μL预冷的-30 ℃乙腈, 涡旋1 min, 12000 r/min离心5 min, 取上清液用于仪器分析。
鹿肉: 取2 g样品于50 mL离心管中加入10 mL乙腈, 涡旋10 min, 超声振荡10 min, 12000 r/min离心5 min, 取上清液。残渣重复1次萃取过程, 合并2次上清液。在40 ℃水浴中氮吹上清液至近干, 加入1 mL乙腈和0.5 mL乙腈饱和的正己烷, 涡旋混匀, 12000 r/min离心5 min, 取200 μL下层溶液于1.5 mL离心管中, 加800 μL水涡旋混匀, 12000 r/min离心5 min后取上清液, 过0.22 μm滤器后用于仪器分析。
1.2.3 标准溶液配制
取乙腈溶解赛拉嗪标准品和内标, 分别得标准和内标工作液(1 μg/mL)。取适量工作液用加入到空白样品中, 随中毒相关样品一同进行前处理, 最终得到赛拉嗪理论质量浓度为0、1、2、5、10、20、50、100 ng/mL的工作标准系列溶液, 用于浓度曲线绘制, 内标质量浓度为20 ng/mL。
1.3 仪器工作条件
QTOF X500R上采用数据依赖采集(information dependent acquisition, IDA)模式对样品萃取物进行非靶向筛查, QTRAP 6500上采用多反应监测(multiple reaction monitoring, MRM)模式进行定量检测。
1.3.1 色谱条件
使用C18色谱柱对组分进行分离, 柱温40 ℃, 进样量5 μL, 流速0.3 mL/min。正离子模式下的流动相为: A相, 2 mmol/L甲酸铵+0.1%甲酸水溶液; B相, 2mmol/L甲酸铵+0.1%甲酸甲醇溶液; 梯度: 0~0.5 min, 5% B; 0.5~3.0 min, 5%~25% B; 3.0~5.5 min, 25%~95% B; 5.5~8.0 min, 95% B; 8.0~8.1 min, 95%~5% B; 8.1~9.0 min, 5% B。负离子模式下的流动相为: A相, 水; B相, 乙腈; 梯度: 0~4.0 min, 5%~70% B; 4.0~5.5 min, 70%~98% B; 5.5~8.0 min, 98% B; 8.0~8.1 min, 98%~5% B; 8.1~9.0 min, 5% B。
1.3.2 质谱条件
非靶向筛查在QTOF X500R上完成, 采用电喷雾正负离子(electrospray ionization, ESI+/-)扫描。离子源温度: 550 ℃; 雾化气和辅助气: 55 psi和60 psi; 气帘气: 30 psi; 离子化电压: 5500 V/-4500 V。对于飞行时间一级离子扫描扫描, 扫描范围: 80~1300 Da; 去簇电压: 80 V/-80 V; 碰撞能: 10 V/-10 V。对于飞行时间二级离子扫描扫描, 扫描范围: 50~1300 Da; 去簇电压: 80 V/-80 V; 碰撞能: (40±20) V/(-40±20) V。
靶向检测在QTRAP 6500上完成, 采用ESI+进行检测。质谱条件与QTOF X500R一致。赛拉嗪的靶向质谱采集参数见表1。
1.3.3 筛查条件与定量方法
依靠数据库对采集数据进行非靶向筛查, 包括: HR-MS/MS libraries of Natural products、Pesticide、Forensic、Mycotoxin、LibView Forensic、Antibiotic、NIST、NIST E＆L。定性标准参考文献[22], 满足3个条件: 与匹配一级离子精确质量数差异小于5 ppm; 与匹配二级质谱表现一致; 保留时间相差小于5%。
样品中赛拉嗪的定量是通过测定与标准品同保留时间的[M+H]+峰的面积, 结合工作曲线、内标回收率与前处理稀释倍数较正后获得。通过向无赛拉嗪残留的样品(n=4)中加入标准品赛拉嗪与内标赛拉嗪-D6, 在避光环境下静置15 min后进行前处理与上机后计算方法的精密度与回收率。
1.4 数据处理
QTOF X500R所采集数据通过AB SCIEX OS 2.2.0软件进行非靶向鉴定并生成图片, QTRAP 6500所采集数据通过AB SCIEX Analyst 1.7软件处理并生成工作曲线, 内标法定量。采用Office Excel 2016和Power Point 2016软件对数据进行统计、制表、绘图处理。分析实验重复6次。
2 结果与分析
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2.1 流行病学调查结果
本次事件共3例病例, 其中2人为父子关系, 1人为员工。3人于2023年8月1日13时30分在某客家汤粉店二楼进食自制的酸菜炒鹿肉、荷兰豆、番薯叶、冬瓜排骨汤等食物, 1人约1 h后出现头痛头晕口干等不适症状, 1人约2 h后出现头痛头晕恶心等不适症状, 1人约4 h后出现头晕、恶心呕吐、伴视物旋转等不适症状, 分别于8月1日20时、22时到医院就诊, 临床查血常规、急凝血、血生化指标如表2所示(仅异常项)。病例自诉鹿肉为网购且冷冻储存, 其余食材为新鲜采购, 由此排除因储存不当导致的微生物或亚硝酸盐中毒的可能。番薯叶、冬瓜、排骨、荷兰豆为常见食材, 导致中毒的可能性较小, 且病例否认有药物与毒物暴露史, 因此初步判定为疑似鹿肉引起的中毒事件, 采集事发当天病例血液、食用的炒鹿肉、生鹿肉样本, 送实验室检测。
2.2 非靶向筛查分析
经筛查, 在生鹿肉、炒鹿肉以及血液中均发现赛拉嗪, 且精确质量数差异均小于5 ppm(表3)。
赛拉嗪在样本中的保留时间、一级质谱信息、二级质谱信息如图1~3所示。在不同样本均能检测到赛拉嗪在ESI源中电离生成的一级离子([C12H16N2S+H]+, m/z 221.11)及其同位素产物一级离子([C12H15N2SD+H]+, m/z 222.11与[C12H14N2SD2+H]+, m/z 223.11)的信号, 同时碎裂后产生的主要特征碎片也与质谱数据库中的二级谱图记录高度匹配。赛拉嗪在炒鹿肉中保留时间为2.515 min, 生鹿肉2.633 min, 病人1血液2.636 min, 与标准品和空白基质加标中的保留时间2.626 min一致(图4)。
2.3 赛拉嗪的预测裂解规律
如图5所示, 赛拉嗪电离后在不同位置的苯环、碳氮键、碳硫键等路径(红色箭头)进行断裂, 生成主要二级离子碎片: C9H11NS+、C9H11N2+、C6H12NS+、C8H10N+、C8H9+、C6H4N+, 与高丰度的二级碎片离子峰相比, 相对丰度超20%的离子碎片与对应的预测分子式分析见表4。
2.4 赛拉嗪的定量分析
在定量分析中, 赛拉嗪在鹿肉中的检出限(limit of detection, LOD)为0.012 μg/kg, 血清中LOD为0.006 ng/mL。方法的精密度与回收率等参数见表5。赛拉嗪在线性范围(1~100 ng/mL)内线性关系良好(r≥0.9993), 经测定赛拉嗪在3例病患血清的含量分别为47.0、16.0和15.6 ng/mL, 未食用的生鹿肉中含量为3.0 μg/kg, 炒鹿肉中含量为395.9 μg/kg。
3 讨论与结论
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赛拉嗪是一种α2-肾上腺素受体激动剂, 具有镇静、镇痛、松弛肌肉的效果, 与可乐定、乐非西定等药物相类似[23], 最初是作为一种降压药被研发, 但后续因为其引发抑郁症的不良作用而被禁止用于人类治疗用途[23-24]。在我国, 赛拉嗪常被用为兽药, GB 31650—2019《食品安全国家标准 食品中兽药最大残留限量》要求在哺乳期动物产品中不得检出赛拉嗪, 而在牛、马中则没有设置残留限量, 对于其他动物产品没有作规定。赛拉嗪在鹿养殖业中被用于采集鹿茸时鹿匹的镇痛, 目前报道的鹿肉赛拉嗪中毒事件主要都聚集在鹿养殖产业兴盛的西北地区[25-26], 但随着冷链运输技术的发展, 南方地区的暴露风险也在不断提高, 像本研究的事件便发生在南方地区。
赛拉嗪过量会导致病例出现意识不清、心率以及血压下降, 并伴随呼吸频率下降以及恶心呕吐等肠胃问题[27-28]。在有关报道中, 病人食用含有赛拉嗪的肉类半小时后出现嗜睡、口干、头晕的症状以及低钾血症[25], 与本研究病人1的中毒症状相同(表现低钾、头晕的症状), 但病人1未表现出嗜睡症状, 在临床症状和流行病学调查研究中并不能很好地与赛拉嗪中毒特征相匹配, 这也是本案件后续采用质谱筛查鉴定手段的最主要原因。通过质谱仪器分析确定鹿肉样本中含有赛拉嗪, 且含量介于已报道血液含量之间(4.8~5000 ng/mL)[25-26]。考虑到赛拉嗪在动物和人类的代谢速度较快, 在人类体内11 h能被完全代谢(动物中则有2~3 h的半衰期)[25-26], 由于不确定其他报道中样本的采集时间, 因此不同事件的病例生物样本不具备可比性, 但考虑到检出的生鹿肉与熟鹿肉中赛拉嗪含量(3.0 μg/kg和395.9 μg/kg)远低于以往报道的生熟鹿肉(193.0 μg/g和5.0 mg/kg)[25-26], 说明本次事件中赛拉嗪暴露水平并不高, 而低剂量的赛拉嗪暴露可能不会引发明显的中枢抑制[29]。此类中毒症状不典型的事件对于临床诊断与流调的误导性很强, 因此十分依赖高分辨质谱等筛查手段对中毒成因进行确证。在确定毒因后, 病例经对症支持治疗, 包括快速静脉补液、氧气吸入、密切监测等手段后已顺利康复出院, 预后均良好。
除此之外, 炒鹿肉中赛拉嗪浓度值远高于生鹿肉的结果也与以往研究发现相似[25-26]。这可能是炒制的过程中赛拉嗪大量从鹿肉富集至食用油中, 而在采样的时候未对熟鹿肉和油进行区分所导致的, 该结果也提示采样人员在采集样本和信息时需做到细致多方位, 以避免信息的遗漏。
近几年, 赛拉嗪被看作是一种新型成瘾药物在美国等国家被广泛使用[30]。尽管食物残留导致赛拉嗪中毒在中国仍较罕见, 但考虑到其对人体造成的危害性与成瘾性, 肉用动物中赛拉嗪的动物种类与施药许可水平、频次等问题可能需要更深层次的研究与探讨。
基金
收起
  • 深圳市医学重点学科建设经费资助项目(SZXK066)
  • 国际原子能机构项目(24959)
文献
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2025年第16卷第16期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250415002
  • 接收时间：2025-04-15
  • 首发时间：2026-01-13
  • 出版时间：2025-08-25
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  • 收稿日期：2025-04-15
基金
深圳市医学重点学科建设经费资助项目(SZXK066)
国际原子能机构项目(24959)
作者信息
    1 深圳市疾病预防控制中心, 深圳 518055
    2 深圳市光明区疾病预防控制中心, 深圳 518106

通讯作者:

* 马浩嘉(1992—), 男, 博士, 主要研究方向为突发应急事件中毒成因检测分析以及食品安全风险监测。E-mail:
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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