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Article(id=1228016572137140478, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1228016566646801206, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202503476, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1742832000000, receivedDateStr=2025-03-25, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1770711566241, onlineDateStr=2026-02-10, pubDate=1758729600000, pubDateStr=2025-09-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1770711566241, onlineIssueDateStr=2026-02-10, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1770711566241, creator=13701087609, updateTime=1770711566241, updator=13701087609, issue=Issue{id=1228016566646801206, tenantId=1146029695717560320, journalId=1227665162245664772, year='2025', volume='52', issue='18', pageStart='3265', pageEnd='3456', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1770711564932, creator=13701087609, updateTime=1770711815039, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1228017615784833769, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1228016566646801206, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1228017615784833770, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1228016566646801206, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=3337, endPage=3340, ext={EN=ArticleExt(id=1228016572904698163, articleId=1228016572137140478, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Detection of fishery anesthetics residues in commonly marketed fresh and live freshwater fish and shrimp, Shandong, 2021-2023, columnId=1228016572783063333, journalTitle=Modern Preventive Medicine, columnName=Nutrition and Food Hygiene, runingTitle=null, highlight=null, articleAbstract=
Objective

To investigate and to analyze the residue status of fishery anesthetics in commonly marketed fresh and live freshwater fish and shrimp in Shandong Province.

Methods

From 2021 to 2023, a total of 480 freshwater fish and shrimp were collected from 16 prefecture-level cities in Shandong Province, and the four anesthetics of eugenol, MS-222, diazepam, and oxazepam were detected by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

Results

Among the four anesthetics, eugenol had the highest detection rate of 31.9% (153/480), followed by diazepam and oxazepam with detection rates of 6.7% (32/480) and 3.1% (15/480), and MS-222 was not detected. Eugenol had the highest detection rate and level of detection in grass carp, diazepam was detected only in fish and oxazepam was detected only in shrimp.

Conclusion

The primary fishery anesthetic detected in commonly marketed fresh and live freshwater fish and shrimp in Shandong Province is eugenol, with overall low residue levels.

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目的

调查分析山东省市售鲜活淡水鱼虾中渔用麻醉剂的残留状况。

方法

2021—2023年在山东省16个地级市共采集480份淡水鱼虾，采用超高效液相色谱串联质谱法对丁香酚、MS-222、地西泮、奥沙西泮4种麻醉剂进行检测。

结果

4种麻醉剂中丁香酚检出率最高，检出率为31.9%（153/480），其次为地西泮和奥沙西泮，检出率分别为6.7%（32/480）和3.1%（15/480），MS-222未检出。丁香酚在草鱼中的检出率和检出含量最高，地西泮仅在鱼类中检出，奥沙西泮仅在虾类中检出。

结论

山东省市售鲜活淡水鱼虾中渔用麻醉剂主要为丁香酚，残留情况整体较轻。

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韩海燕，E-mail:
, copyrightStatement=本刊刊出的所有文章不代表中华预防医学会和本刊编委会的观点，除非特别声明。, copyrightOwner=中华预防医学会和四川大学华西公共卫生学院, extLink=null, articleAbsUrl=null, sourceXml=o2Jk2o1kUnJPYSstNfk4nA==, magXml=s5552CjbjiTFh8c260xyRA==, pdfUrl=null, pdf=v7rmAHUiBwejpl0pF8VDAw==, pdfFileSize=676516, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=xarb/x+Ev+HJc/q6UWDaFA==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=NpzKVgMCeJzdvIyITgwj8A==, mapNumber=null, authorCompany=null, fund=null, authors=

朱颖(1993—)，女，本科，主管技师，研究方向：食品安全与理化检验

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朱颖(1993—)，女，本科，主管技师，研究方向：食品安全与理化检验

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朱颖(1993—)，女，本科，主管技师，研究方向：食品安全与理化检验

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Journal of Hygiene Research, 2025, 54(1): 129-135.(In Chinese), articleTitle=Determination of diazepam and its three metabolites in fish by pass-through solid phase extraction purification combined with ultra-perfor-mance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1228016584065740877, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=5, pageStart=52, pageEnd=59, url=null, language=null, rfNumber=[20], rfOrder=38, authorNames=陈旭晋, 陆宇阳, 苑华宁, journalName=农产品质量与安全, refType=null, unstructuredReference=陈旭晋，陆宇阳，苑华宁，等．华东某地区养殖淡水鱼中地西泮残留风险分析及来源调查[J].农产品质量与安全，2024(5):52-59., articleTitle=华东某地区养殖淡水鱼中地西泮残留风险分析及来源调查, refAbstract=null), Reference(id=1228016584195764305, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=5, pageStart=52, pageEnd=59, url=null, language=null, rfNumber=[20], rfOrder=39, authorNames=Chen XJ, Lu YY, Yuan HN, journalName=Quality and Safety of Agro-Products, refType=null, unstructuredReference=Chen XJ, Lu YY, Yuan HN, et al. 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Advances in thesafety research of fish anesthetics[J]. Chinese Fishery Quality and Standards, 2013, 3(2): 24-28.(In Chinese), articleTitle=Advances in thesafety research of fish anesthetics, refAbstract=null), Reference(id=1228016584585834597, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, doi=null, pmid=null, pmcid=null, year=2025, volume=42, issue=1, pageStart=69, pageEnd=71, url=null, language=null, rfNumber=[22], rfOrder=42, authorNames=林文池, 朱悦君, 杨芳, journalName=环境与健康杂志, refType=null, unstructuredReference=林文池，朱悦君，杨芳，等．粤东某市市售水产品海鱼和虾中渔用休眠诱导剂的残留水平及污染特征分析[J].环境与健康杂志，2025, 42(1): 69-71., articleTitle=粤东某市市售水产品海鱼和虾中渔用休眠诱导剂的残留水平及污染特征分析, refAbstract=null), Reference(id=1228016584699080811, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, doi=null, pmid=null, pmcid=null, year=2025, volume=42, issue=1, pageStart=69, pageEnd=71, url=null, language=null, rfNumber=[22], rfOrder=43, authorNames=Lin WC, Zhu YJ, Yang F, journalName=Journal of Environment and Health, refType=null, unstructuredReference=Lin WC, Zhu YJ, Yang F, et al.Analysis of the residual level and pollution characteristics of fish sleep inducers in sea fish and shrimp sold in a city in eastern Guangdong[J]. Journal of Environment and Health, 2025, 42(1): 69-71.(In Chinese), articleTitle=Analysis of the residual level and pollution characteristics of fish sleep inducers in sea fish and shrimp sold in a city in eastern Guangdong, refAbstract=null)], funds=[Fund(id=1228016579321983779, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, awardId=2024NYNS018, language=CN, fundingSource=济宁市重点研发计划(2024NYNS018), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1228016574167183763, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, xref=null, ext=[AuthorCompanyExt(id=1228016574175572372, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, companyId=1228016574167183763, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Jining Center for Disease Control and Prevention, Jining, Shandong 272000, China), AuthorCompanyExt(id=1228016574183960981, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, companyId=1228016574167183763, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=济宁市疾病预防控制中心理化检验科，山东　济宁　272000)])], figs=[ArticleFig(id=1228016578009166524, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=EN, label=Fig.1, caption=Detection status of eugenol and diazepam in freshwater fish from different cities, figureFileSmall=V4yeGtoFj9VDEVa6+q+yfA==, figureFileBig=xarb/x+Ev+HJc/q6UWDaFA==, tableContent=null), ArticleFig(id=1228016578155967179, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=CN, label=图1, caption=不同地市淡水鱼中丁香酚和地西泮的检出情况, figureFileSmall=V4yeGtoFj9VDEVa6+q+yfA==, figureFileBig=xarb/x+Ev+HJc/q6UWDaFA==, tableContent=null), ArticleFig(id=1228016578508288736, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=EN, label=Table 1, caption=

Average recovery rate and precision of the method(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
检测项目添加水平（μg/kg）平均回收率（%）RSD（%）
丁香酚491.84.51
5089.62.52
200102.72.04
MS-2221.483.35.98
5100.43.48
2092.32.63
地西泮198.32.28
586.31.63
2096.11.10
奥沙西泮1102.22.91
588.71.52
2095.91.13
), ArticleFig(id=1228016578663477993, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=CN, label=表1, caption=

方法的平均回收率及精密度（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
检测项目添加水平（μg/kg）平均回收率（%）RSD（%）
丁香酚491.84.51
5089.62.52
200102.72.04
MS-2221.483.35.98
5100.43.48
2092.32.63
地西泮198.32.28
586.31.63
2096.11.10
奥沙西泮1102.22.91
588.71.52
2095.91.13
), ArticleFig(id=1228016578789307125, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=EN, label=Table 2, caption=

Residues of fishery anesthetics in commonly marketed fresh and live freshwater fish and shrimp in Shandong Province

, figureFileSmall=null, figureFileBig=null, tableContent=
检测项目样品份数检出样品数检出率
（%）		平均值
（μg/kg）
丁香酚48015331.9193.8
MS-22248000.0ND
地西泮480326.70.7
奥沙西泮480153.10.8
), ArticleFig(id=1228016578927719168, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=CN, label=表2, caption=

山东省市售鲜活淡水鱼虾中渔用麻醉剂残留情况

, figureFileSmall=null, figureFileBig=null, tableContent=
检测项目样品份数检出样品数检出率
（%）		平均值
（μg/kg）
丁香酚48015331.9193.8
MS-22248000.0ND
地西泮480326.70.7
奥沙西泮480153.10.8
), ArticleFig(id=1228016579045159685, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=EN, label=Table 3, caption=

Residues of three fishery anesthetics in different freshwater fish and shrimps

, figureFileSmall=null, figureFileBig=null, tableContent=
种类品种样本数
（份）		丁香酚地西泮奥沙西泮
检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)		检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)		检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)
鱼类鲤鱼1766939.2175.64 9522514.21.121.900.0NDND
草鱼714563.4654.612 61434.20.65.800.0NDND
鲫鱼591728.885.52 52011.70.50.900.0NDND
黑鱼1915.391.31 72800.0NDND00.0NDND
鲶鱼17847.1306.22 76700.0NDND00.0NDND
鲢鱼13323.1131.31 28200.0NDND00.0NDND
鲟鱼13538.576.945117.70.50.800.0NDND
黄颡鱼11436.468.957700.0NDND00.0NDND
鲈鱼1100.0NDND218.21.04.500.0NDND
罗非鱼1000.0NDND00.0NDND00.0NDND
合计40015238.0232.112 614328.00.821.900.0NDND
虾类小龙虾4200.0NDND00.0NDND49.52.357.3
河虾3812.64.415500.0NDND1128.92.328.2
合计8011.32.215500.0NDND1518.82.357.3
), ArticleFig(id=1228016579154211599, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1228016572137140478, language=CN, label=表3, caption=

3种渔用麻醉剂在不同淡水鱼虾中的残留情况

, figureFileSmall=null, figureFileBig=null, tableContent=
种类品种样本数
（份）		丁香酚地西泮奥沙西泮
检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)		检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)		检出数
（份）		检出率
（%）		平均值
(μg/kg)		最大值
(μg/kg)
鱼类鲤鱼1766939.2175.64 9522514.21.121.900.0NDND
草鱼714563.4654.612 61434.20.65.800.0NDND
鲫鱼591728.885.52 52011.70.50.900.0NDND
黑鱼1915.391.31 72800.0NDND00.0NDND
鲶鱼17847.1306.22 76700.0NDND00.0NDND
鲢鱼13323.1131.31 28200.0NDND00.0NDND
鲟鱼13538.576.945117.70.50.800.0NDND
黄颡鱼11436.468.957700.0NDND00.0NDND
鲈鱼1100.0NDND218.21.04.500.0NDND
罗非鱼1000.0NDND00.0NDND00.0NDND
合计40015238.0232.112 614328.00.821.900.0NDND
虾类小龙虾4200.0NDND00.0NDND49.52.357.3
河虾3812.64.415500.0NDND1128.92.328.2
合计8011.32.215500.0NDND1518.82.357.3
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2021—2023年山东省市售鲜活淡水鱼虾中渔用麻醉剂残留检测
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朱颖 , 柴玲玉 , 聂重重 , 贾瑞 , 韩海燕
现代预防医学 | 营养与食品卫生 2025,52(18): 3337-3340
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现代预防医学 | 营养与食品卫生 2025, 52(18): 3337-3340
2021—2023年山东省市售鲜活淡水鱼虾中渔用麻醉剂残留检测
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朱颖, 柴玲玉, 聂重重, 贾瑞, 韩海燕
作者信息
  • 济宁市疾病预防控制中心理化检验科，山东　济宁　272000

    • 朱颖(1993—)，女，本科，主管技师，研究方向：食品安全与理化检验

通讯作者:

韩海燕，E-mail:
Detection of fishery anesthetics residues in commonly marketed fresh and live freshwater fish and shrimp, Shandong, 2021-2023
Ying ZHU, Ling-yu CHAI, Chong-chong NIE, Rui JIA, Hai-yan HAN
Affiliations
  • Jining Center for Disease Control and Prevention, Jining, Shandong 272000, China
出版时间: 2025-09-25 doi: 10.20043/j.cnki.MPM.202503476
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摘要
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目的

调查分析山东省市售鲜活淡水鱼虾中渔用麻醉剂的残留状况。

方法

2021—2023年在山东省16个地级市共采集480份淡水鱼虾，采用超高效液相色谱串联质谱法对丁香酚、MS-222、地西泮、奥沙西泮4种麻醉剂进行检测。

结果

4种麻醉剂中丁香酚检出率最高，检出率为31.9%（153/480），其次为地西泮和奥沙西泮，检出率分别为6.7%（32/480）和3.1%（15/480），MS-222未检出。丁香酚在草鱼中的检出率和检出含量最高，地西泮仅在鱼类中检出，奥沙西泮仅在虾类中检出。

结论

山东省市售鲜活淡水鱼虾中渔用麻醉剂主要为丁香酚，残留情况整体较轻。

淡水鱼虾  /  渔用麻醉剂  /  残留
Objective

To investigate and to analyze the residue status of fishery anesthetics in commonly marketed fresh and live freshwater fish and shrimp in Shandong Province.

Methods

From 2021 to 2023, a total of 480 freshwater fish and shrimp were collected from 16 prefecture-level cities in Shandong Province, and the four anesthetics of eugenol, MS-222, diazepam, and oxazepam were detected by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

Results

Among the four anesthetics, eugenol had the highest detection rate of 31.9% (153/480), followed by diazepam and oxazepam with detection rates of 6.7% (32/480) and 3.1% (15/480), and MS-222 was not detected. Eugenol had the highest detection rate and level of detection in grass carp, diazepam was detected only in fish and oxazepam was detected only in shrimp.

Conclusion

The primary fishery anesthetic detected in commonly marketed fresh and live freshwater fish and shrimp in Shandong Province is eugenol, with overall low residue levels.

Freshwater fish and shrimp  /  fishery anesthetics  /  Residue
朱颖, 柴玲玉, 聂重重, 贾瑞, 韩海燕. 2021—2023年山东省市售鲜活淡水鱼虾中渔用麻醉剂残留检测. 现代预防医学, 2025 , 52 (18) : 3337 -3340 . DOI: 10.20043/j.cnki.MPM.202503476
Ying ZHU, Ling-yu CHAI, Chong-chong NIE, Rui JIA, Hai-yan HAN. Detection of fishery anesthetics residues in commonly marketed fresh and live freshwater fish and shrimp, Shandong, 2021-2023[J]. Modern Preventive Medicine, 2025 , 52 (18) : 3337 -3340 . DOI: 10.20043/j.cnki.MPM.202503476
正文
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随着生活水平的提升，人们愈发注重食品的新鲜程度，在鱼虾等水产品的养殖和运输中，常使用麻醉剂来保证其鲜活度[1]。渔用麻醉剂可以降低鱼虾的应激反应，减少死亡和受伤几率，但要合理使用，不然残留的麻醉剂会通过食物链传递给人类，对人体健康造成影响[2]。
渔用麻醉剂约有30余种，包括丁香酚、3-氨基苯甲酸乙酯甲基磺酸盐（MS-222）、2-苯氧乙醇和二氧化碳等，其中，丁香酚和MS-222应用最为广泛[3]。丁香酚是从丁香中提取的天然植物源麻醉剂，具备抗菌、抗氧化以及镇痛麻醉的作用，因其价格低、效果好、复苏快等特点在水产品运输和保鲜领域应用广泛[4]。美国毒理部曾指出丁香酚具有肝毒性，对肝脏有一定的损伤[5]。欧洲食品安全局认为丁香酚对皮肤和眼睛具有刺激作用，接触后会产生过敏反应[6]。MS-222是经过美国食品和药品管理局认可的相对安全的渔用麻醉剂，但仍具有轻微毒性，必须休眠21天后才允许在市场上销售[7]。目前, 我国尚未制定水产品中丁香酚、MS-222的使用规范，其潜在的药物残留隐患成为公众健康领域关注的焦点。
地西泮是抗焦虑、抗惊厥药物，对人体具有抗焦虑、镇静催眠的功效，对于水生动物则有降低新陈代谢，控制活动减少应激反应等作用，属于国家管制的二类精神药品[8]。GB 31650—2019《食品安全国家标准食品中兽药最大残留限量》中明确规定，地西泮不得在动物性食品中检出。然而四川、天津、重庆、北京等多地市售淡水鱼中仍存在地西泮残留超标现象[9]。地西泮的代谢主要是在肝脏进行，代谢产物共5～6种，其中主要代谢物为奥沙西泮[10]。长期食用地西泮和奥沙西泮残留量较大的水产品，会对人体健康产生潜在的风险和危害，特别是对儿童、孕妇、老年人和患有心血管等疾病的慢性病患者，可能对人体造成不可预期的危害[11]。因此有必要对山东省水产品中的地西泮及其代谢物奥沙西泮进行检测。
山东省作为人口大省和渔业大省，水产品食用消费鲜重总量位居全国第四位，高达315.66万吨[12]。然而，目前关于渔用麻醉剂在山东省淡水鱼虾中的残留状况尚未见系统地研究报道。为此，本研究历时3年，在常规淡水鱼监测的基础上，新增河虾、小龙虾等特色品种，累计采集样品480份。监测项目不仅包含丁香酚和MS-222两种常用的渔用麻醉剂，还将限制使用药物地西泮及其代谢物奥沙西泮纳入监测范围，旨在获得更全面的数据，为相关部门对水产品中渔用麻醉剂的管理提供数据支撑。
1　材料与方法
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1.1　样品采集与制备
2021—2023年在山东省16个地市，随机采集商店、农贸市场销售的鲜活鲤鱼、草鱼、鲫鱼、黑鱼、鲢鱼、鲟鱼、黄颡鱼、罗非鱼、鲶鱼、鲈鱼、小龙虾、河虾12种市场销量高的品种，共计480份。样品制备依种类分别进行，对于鱼类，去头、骨、内脏，取肌肉等可食部位绞碎混合均匀；对于虾类则在清洗后，去掉虾头、虾皮、肠腺，得到整条虾肉绞碎混合均匀。
1.2　试剂
丁香酚标准品、MS-222标准品购于德国 Dr.Ehrenstorfer，丁香酚-d3购于ISOREAG，地西泮标准品、奥沙西泮标准品、地西泮-d5、奥沙西泮-d5均购于天津阿尔塔科技有限公司。
乙腈、甲醇、甲酸均为色谱纯，购于德国默克；无水硫酸钠、氯化钠均为分析纯，购于科密欧化学试剂有限公司。
1.3　仪器和设备
超高效液相色谱-三重四极杆串联质谱仪（TQ-S，美国waters公司），高速冷冻离心机（Multifuge X1R，美国Thermo公司）， 电子天平（MS204TS，梅特勒托利多公司），氮吹仪（AUTO EVA，Reeko睿科公司），Sep-Pak C18 固相萃取柱（500 mg，3 ml，美国Waters公司），Oasis PRiME HLB 固相萃取柱（200 mg/6 ml，美国Waters公司）。
1.4　检测方法
参照2021年国家食品污染物和有害因素风险监测手册进行[13] 。
1.5　数据统计分析
采用Excel 2021表录入本次淡水鱼虾中4种麻醉剂的检出数据，用SPSS 25. 0对所录入数据进行分析和χ2检验，检验水准α=0.05。对未检出数据的处理，样本中未检出数据的比例>60%时，所有未检出数据用检出限（LOD）替代；未检出数据的比例<60%时，所有未检出数据用50% LOD替代[14]。
2　结果与分析
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2.1　方法学评价
以丁香酚、MS-222、地西泮、奥沙西泮的浓度为横坐标，以目标物和内标物的峰面积之比作为纵坐标，拟合线性方程，结果显示4种目标化合物方法曲线的线性均良好（R>0.999）。当称样量为5 g时，丁香酚的检出限为0.3 μg/kg，MS-222的检出限为0.14 μg/kg；当称样量为2 g时，地西泮和奥沙西泮的检出限均为0.5 μg/kg。
取空白鱼肉基质分别进行低、中、高3个不同浓度水平的加标回收实验，每个添加水平重复测定6次，平均回收率及精密度见表1。
2.2　总体检出情况
本研究共采集样品480份，其中153份样品中检出丁香酚，检出率为31.9%（153/480），检出值中最低为3.07 μg/kg，最高为12 614 μg/kg；检出值在LOD~100 μg/kg范围内的为71份，占总检出份数的46.4%（71/153）；检出值在100~1 000 μg/kg范围内的为54份，占总检出份数的35.3%（54/153）；检出值在1 000~5 000 μg/kg范围内的为26份，占总检出份数的17%（26/153）；检出值在5 000 μg/kg以上的为2份，占总检出份数的1.3%（2/153）。地西泮的检出率为6.7%（32/480），检出值中最低为0.59 μg/kg，最高为21.9 μg/kg。奥沙西泮的检出率为3.1%（15/480），检出值中最低为1.07 μg/kg，最高为57.3 μg/kg。研究发现480份样品均未检出MS-222。4种麻醉剂中仅有地西泮有国家限量标准，因此只评价地西泮的超标情况，地西泮检出即为超标，超标率为6.7%（32/480）。详细情况见表2。
2.3　不同种类结果分析
丁香酚在鱼类和虾类中均有检出，鱼类的检出率远高于虾类，10个品种的鱼中仅有鲈鱼和罗非鱼未检出，其余均有检出，其中草鱼的检出率和检出含量最高，检出率为63.4%（45/71），检出范围为7.26~12 614 μg/kg；虾类中仅有一份河虾中检出丁香酚，小龙虾中未被检出。地西泮仅在鱼类中检出，虾类中未被检出，其中鲤鱼的检出率和检出含量最高，检出率为14.2%（25/176），检出范围为0.59~21.9 μg/kg。奥沙西泮仅在虾类中检出，鱼类中未被检出，河虾的检出率（28.9%）高于小龙虾（9.5%）。不同品种淡水鱼中丁香酚的检出率差异具有统计学意义（χ2=54.265，P<0.001）。详细情况见表3。
2.4　地域性结果分析
由图1可知，16个地市均有鱼类样品检出丁香酚，滨州、德州、菏泽、济南、济宁、聊城、临沂、日照8个地市的淡水鱼检出地西泮。其中淄博的丁香酚检出率最高，检出率为67%（20/30）；菏泽的地西泮检出率最高，检出率为30%（9/30）。不同地市市售淡水鱼中丁香酚的检出率差异具有统计学意义（χ2=46.505，P<0.001）。
济南、淄博、济宁、泰安、德州、聊城、临沂、菏泽8个地市采集了淡水虾样品，8个地市均检出奥沙西泮，检出率无统计学差异（χ2=10.183，P=0.121）。
3　讨论
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本研究结果显示2021—2023年山东省市售鲜活淡水鱼虾中渔用麻醉剂主要为丁香酚，其总体检出率为31.9%（153/480），与国内其他地区的研究数据（41.13%~89.47%）[15-17]相比，山东省丁香酚检出率处于相对较低水平，可能是由于山东省淡水养殖产业比较发达，无需进行远距离运输，减少了长途运输对麻醉剂的需求。本次监测中，丁香酚残留量跨度较大（3.07~12 614 μg/kg），检出值多数在1 000 μg/kg以下，仅一份草鱼样品中丁香酚残留量高达12 614 μg/kg，虽高于湖北省[15]（2 601 μg/kg）、江西省[16]（7 980 μg/kg），但低于上海市浦东新区[17]的残留最大值（14 464 μg/kg）。
地西泮和奥沙西泮同属苯二氮卓类药物，通过与γ-氨基丁酸受体特异性结合，从而产生中枢神经抑制的作用[18]。鉴于该类药物的潜在安全风险，我国《食品安全国家标准食品中兽药最大残留限量》（GB 31650—2019）以及国际食品法典委员会和欧盟相关法规均明确规定，动物源性食品中不得检出地西泮[19]。2021-2023山东省市售鲜活淡水鱼虾中地西泮的检出率为6.7%，高于柏品清等[17]研究结果（3.51%），但远低于陈旭晋等[20]研究结果（26.8%）。奥沙西泮作为地西泮的代谢物，并未在淡水鱼中检出，仅在淡水虾中检测到，表明在虾类养殖或运输过程中可能存在单独添加奥沙西泮的行为。480份淡水鱼虾样品中均未检出MS-222，这可能与样品来源有关；由于MS-222其价格较高，其主要应用于金鱼、中华鲟、斑马鱼等观赏鱼和经济价值较高的鱼类上[21]，而本次采集样品均为日常食用淡水鱼虾，因此未检出MS-222符合其使用特点。
本次研究发现鱼类和虾类中各麻醉剂使用情况存在显著差异。虾类中丁香酚类化合物的整体检出率和检出量远远低于鱼类，与彭雅丹等[16]研究结果一致，这可能是由于虾类的甲壳外骨骼结构限制了丁香酚的吸收，而鱼类通过鳃器官进行呼吸的过程中，更容易摄入丁香酚，从而导致其体内丁香酚的检出率和检出量相对较高。地西泮仅在鱼类中检出，奥沙西泮仅在虾类中检出，与林文池等[22]研究结果一致，可能是由于地西泮半衰期长更适用于需要长效镇静的鱼类运输；而奥沙西泮作为地西泮的活性代谢物，能够满足虾类等短程运输的需求。由于本次仅采集鱼虾类样品，未涵盖饲料、水体及底泥等样本，因此仅推断为运输过程中药品使用偏好导致的差异，不能全面反映实际情况，下一步将加大监测范围，进一步调查相关原因。同时建议积极推广低温运输、电脉冲麻醉等物理技术，以减少化学麻醉剂的使用。
基金
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  • 济宁市重点研发计划(2024NYNS018)
文献
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2025年第52卷第18期
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doi: 10.20043/j.cnki.MPM.202503476
  • 接收时间：2025-03-25
  • 首发时间：2026-02-10
  • 出版时间：2025-09-25
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  • 收稿日期：2025-03-25
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    济宁市疾病预防控制中心理化检验科，山东　济宁　272000

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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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