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Article(id=1151881496466960840, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250302001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1740844800000, receivedDateStr=2025-03-02, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752559549681, onlineDateStr=2025-07-15, pubDate=1748102400000, pubDateStr=2025-05-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752559549681, onlineIssueDateStr=2025-07-15, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752559549681, creator=13701087609, updateTime=1752559549681, updator=13701087609, issue=Issue{id=1151881493552394994, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='10', 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=0, createTime=1752559548986, creator=13701087609, updateTime=1756202008453, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1167159075906265916, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1167159075906265917, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151881493552394994, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=126, endPage=133, ext={EN=ArticleExt(id=1151923895054512857, articleId=1151881496466960840, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of fish sedatives and quinolones residues in freshwater fish and assessment of dietary exposure risk, columnId=1151923891565326960, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Processing and Quality Safety of Aquatic Products, runingTitle=null, highlight=null, articleAbstract=

Objective To determine the residual levels of fish sedatives and quinolones residues in commercially freshwater fish and evaluate their dietary exposure risk. Methods A total of 77 batches of freshwater fish were collected in 8 administrative regions of Wuhan City. High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used to determine the content of fishing anesthetics (MS-222, benzocaine, eugenol) and quinolone antibiotics (enrofloxacin, ciprofloxacin, ofloxacin, levofloxacin, levofloxacin, norfloxacin), and the dietary exposure risk of each compound was analyzed using a quantitative analysis method. Results MS-222 and benzocaine were not detected in all samples, and 48 batches of eugenol were detected with a content range of 2.59-1927.30 μg/kg, with a failure rate of 29.8%. The dietary exposure risk values for all age groups were less than 0.4%, indicating low dietary risk. All samples did not detect peofloxacin and norfloxacin. Enrofloxacin was detected in 34 batches with a content range of 1.74-5585.00 μg/kg, and ofloxacin was detected in 2 batches with a content range of 36.30-65.60 μg/kg, the overall failure rate was 18.2%, and the dietary exposure risk of all age groups was less than 8.00%. According to species analysis, the content range of enrofloxacin in loaches and yellow catfish was as follows: 2.74-5585.00 μg/kg and 6.82-1014.00 μg/kg, with dietary risks of 55.4% and 9.0%, respectively. Conclusion The fishery anesthetic used in this region is eugenol, which is characterized by high detection rate and large residual amount, and requires the development of normative documents to guide its use. Enrofloxacin, as the main quinolone antibiotic used in the region, has two high-risk species: Loach and yellow catfish. Market regulatory authorities should focus on the supervision of these two species.

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目的 测定市售淡水鱼中渔用麻醉剂和喹诺酮类抗生素的残留含量并评估其膳食暴露风险。方法 在武汉市8个行政区域中共收集77批淡水鱼, 采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分别测定渔用麻醉剂(MS-222、苯佐卡因、丁香酚)及喹诺酮类抗生素(恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星)的含量, 用点评估法分析各化合物的膳食暴露风险。结果 所有样品中均未检出MS-222和苯佐卡因, 检出丁香酚48批次, 含量范围为2.59~1927.30 μg/kg, 不合格率为29.8%, 各年龄段人群膳食暴露风险值均小于0.4%, 膳食风险低。所有样品均未检出培氟沙星和诺氟沙星, 检出恩诺沙星34批, 含量范围为1.74~5585.00 μg/kg, 氧氟沙星2批, 含量范围为36.30~65.60 μg/kg, 总体不合格率为18.2%, 各年龄段人群的膳食暴露风险均小于8.00%。按品种分析, 泥鳅和黄颡鱼中恩诺沙星的含量范围分别为: 2.74~5585.00 μg/kg和6.82~1014.00 μg/kg, 膳食风险分别为: 55.4%和9.0%。结论 该地区使用的渔用麻醉剂为丁香酚, 其特点是检出率高和残留量大, 需要制定规范性文件指导使用。恩诺沙星作为主要的喹诺酮类抗生素药物在该地区使用, 有两个高风险品种: 泥鳅和黄颡鱼, 市场监管部门应重点关注这两个品种的监管。

, correspAuthors=谢柏艳, authorNote=null, correspAuthorsNote=
* 谢柏艳(1982—), 女, 硕士, 主管药师, 主要研究方向食品质量安全研究。E-mail:
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李文博(1989—), 男, 硕士, 主管药师, 主要研究方向为食品质量安全研究。E-mail:

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李文博(1989—), 男, 硕士, 主管药师, 主要研究方向为食品质量安全研究。E-mail:

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Occurrence and health risk assessment of quinolone antibiotics in aquatic products during production and circulation[J]. 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Study on the risk of pesticides and veterinary drug residues in aquaculture environment and their metabolism in aquatic products[D]. Shanghai: Shanghai Ocean University, 2023., articleTitle=null, refAbstract=null)], funds=[Fund(id=1167158514007945972, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, awardId=Hbscjg-KJ2022002, language=CN, fundingSource=湖北省市场监督管理局科技计划项目(Hbscjg-KJ2022002), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1167158510648308372, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, xref=null, ext=[AuthorCompanyExt(id=1167158510652502677, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, companyId=1167158510648308372, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Wuhan Institute for Drug and Medical Device Control, Wuhan 430075, China), AuthorCompanyExt(id=1167158510656696982, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, companyId=1167158510648308372, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=武汉药品医疗器械检验所, 武汉 430075)])], figs=[ArticleFig(id=1167158512237949640, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Fig.1, caption=Dietary risk of enrofloxacin in different species of fish, figureFileSmall=zLXwfEy1nE9giZWhfAuozA==, figureFileBig=BieM8CgIvBST80xHx8madA==, tableContent=null), ArticleFig(id=1167158512309252810, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=图1, caption=不同品种鱼类中恩诺沙星的膳食风险, figureFileSmall=zLXwfEy1nE9giZWhfAuozA==, figureFileBig=BieM8CgIvBST80xHx8madA==, tableContent=null), ArticleFig(id=1167158512355390156, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 1, caption=

Standard curve equations, LODs, LOQs, recoveries and RSDs of quinolone antibiotics (n=3)

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 线性方程 线性范围/(μg/L) LODs
/(μg/kg)		 LOQs
/(μg/kg)		 回收率/% (RSDs/%)
4 μg/kg 8 μg/kg 20 μg/kg
环丙沙星 Y=0.0222X+0.0208 5.1~202.8 0.04 0.13 71.1 (7.2) 82.9 (5.8) 79.1 (3.1)
恩诺沙星 Y=0.0178X-0.0133 5.1~202.6 0.02 0.08 104.5 (6.4) 104.9 (4.2) 95.8 (2.3)
诺氟沙星 Y=0.0144X-0.00181 5.2~211.0 0.04 0.14 82.1 (6.3) 80.1 (4.1) 81.7 (2.5)
培氟沙星 Y=0.0301X+0.0395 3.8~152.3 0.02 0.07 104.6 (4.3) 103.9 (3.2) 110.4 (2.7)
氧氟沙星 Y=0.0439X-0.0439 5.2~207.6 0.03 0.09 104.0 (6.9) 86.8 (4.9) 87.9 (3.4)
), ArticleFig(id=1167158512443470542, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表1, caption=

喹诺酮类抗生素的标准曲线方程、LODs、LOQs、回收率及RSDs (n=3)

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 线性方程 线性范围/(μg/L) LODs
/(μg/kg)		 LOQs
/(μg/kg)		 回收率/% (RSDs/%)
4 μg/kg 8 μg/kg 20 μg/kg
环丙沙星 Y=0.0222X+0.0208 5.1~202.8 0.04 0.13 71.1 (7.2) 82.9 (5.8) 79.1 (3.1)
恩诺沙星 Y=0.0178X-0.0133 5.1~202.6 0.02 0.08 104.5 (6.4) 104.9 (4.2) 95.8 (2.3)
诺氟沙星 Y=0.0144X-0.00181 5.2~211.0 0.04 0.14 82.1 (6.3) 80.1 (4.1) 81.7 (2.5)
培氟沙星 Y=0.0301X+0.0395 3.8~152.3 0.02 0.07 104.6 (4.3) 103.9 (3.2) 110.4 (2.7)
氧氟沙星 Y=0.0439X-0.0439 5.2~207.6 0.03 0.09 104.0 (6.9) 86.8 (4.9) 87.9 (3.4)
), ArticleFig(id=1167158512506385104, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 2, caption=

Standard curve equations, LODs, LOQs, recoveries and RSDs of fish sedatives (n=3)

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 线性方程 线性范围
/(μg/L)		 LODs
/(μg/kg)		 LOQs
/(μg/kg)		 回收率/% (RSDs/%)
10 μg/kg 25 μg/kg 50 μg/kg
MS-222 Y=1.95×104X+2.55×103 5.1~100.3 0.16 0.53 90.6 (6.1) 95.1 (3.8) 97.6 (2.2)
苯佐卡因 Y=2.5×104X+1.32×103 5.2~100.5 0.12 0.41 108.3 (7.3) 100.2 (5.1) 106.5 (3.1)
丁香酚 Y=741X-862 5.1~100.3 0.51 1.67 95.2 (5.8) 93.7 (3.8) 96.3 (2.5)
), ArticleFig(id=1167158512636408530, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表2, caption=

渔用麻醉剂的标准曲线方程、LODs、LOQs、回收率及RSDs (n=3)

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 线性方程 线性范围
/(μg/L)		 LODs
/(μg/kg)		 LOQs
/(μg/kg)		 回收率/% (RSDs/%)
10 μg/kg 25 μg/kg 50 μg/kg
MS-222 Y=1.95×104X+2.55×103 5.1~100.3 0.16 0.53 90.6 (6.1) 95.1 (3.8) 97.6 (2.2)
苯佐卡因 Y=2.5×104X+1.32×103 5.2~100.5 0.12 0.41 108.3 (7.3) 100.2 (5.1) 106.5 (3.1)
丁香酚 Y=741X-862 5.1~100.3 0.51 1.67 95.2 (5.8) 93.7 (3.8) 96.3 (2.5)
), ArticleFig(id=1167158512716100309, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 3, caption=

Detection results of fish sedatives

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
MS-222 77 未检出 / / / / /
苯佐卡因 77 未检出 / / / / /
丁香酚 77 48 62.3 2.59~1927.30 143.10 23 29.8
), ArticleFig(id=1167158512841929432, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表3, caption=

渔用麻醉剂的检出结果

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
MS-222 77 未检出 / / / / /
苯佐卡因 77 未检出 / / / / /
丁香酚 77 48 62.3 2.59~1927.30 143.10 23 29.8
), ArticleFig(id=1167158512950981338, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 4, caption=

Detection results of eugenol in different species

, figureFileSmall=null, figureFileBig=null, tableContent=
品种 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
草鱼 15 14 93.3 9.77~1927.30 372.00 9 60.0
黄颡鱼 12 9 75.0 10.38~247.70 43.50 3 25.0
鲫鱼 12 8 66.7 7.71~444.30 80.40 3 25.0
鲈鱼 7 3 42.9 9.77~283.00 45.20 1 14.3
泥鳅 8 3 37.5 2.59~463.20 58.80 1 12.5
翘嘴鲌 3 2 66.7 7.16~1423.10 476.70 1 33.3
鳝鱼 6 2 33.3 11.30~28.50 6.63 0 0.0
鳙鱼 10 4 40.0 12.50~427.90 58.20 2 20.0
鳊鱼 4 3 75.0 256.30~473.40 277.40 3 75.0
), ArticleFig(id=1167158513101976285, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表4, caption=

不同品种中丁香酚的检出结果

, figureFileSmall=null, figureFileBig=null, tableContent=
品种 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
草鱼 15 14 93.3 9.77~1927.30 372.00 9 60.0
黄颡鱼 12 9 75.0 10.38~247.70 43.50 3 25.0
鲫鱼 12 8 66.7 7.71~444.30 80.40 3 25.0
鲈鱼 7 3 42.9 9.77~283.00 45.20 1 14.3
泥鳅 8 3 37.5 2.59~463.20 58.80 1 12.5
翘嘴鲌 3 2 66.7 7.16~1423.10 476.70 1 33.3
鳝鱼 6 2 33.3 11.30~28.50 6.63 0 0.0
鳙鱼 10 4 40.0 12.50~427.90 58.20 2 20.0
鳊鱼 4 3 75.0 256.30~473.40 277.40 3 75.0
), ArticleFig(id=1167158513177473760, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 5, caption=

Dietary risk assessment of eugenol

, figureFileSmall=null, figureFileBig=null, tableContent=
人群 体重/kg 摄入量/(g/d) ADI/[mg/(kg·bw)] 平均残留含量/(μg/kg) 最高残留含量/(μg/kg) 平均RQ/% 最高RQ/%
儿童 20 40 1.0 143.1 1927.3 0.03 0.39
成人 60 80 1.0 143.1 1927.3 0.02 0.26
老年人 60 50 1.0 143.1 1927.3 0.01 0.16
), ArticleFig(id=1167158513236194018, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表5, caption=

丁香酚的膳食风险评估

, figureFileSmall=null, figureFileBig=null, tableContent=
人群 体重/kg 摄入量/(g/d) ADI/[mg/(kg·bw)] 平均残留含量/(μg/kg) 最高残留含量/(μg/kg) 平均RQ/% 最高RQ/%
儿童 20 40 1.0 143.1 1927.3 0.03 0.39
成人 60 80 1.0 143.1 1927.3 0.02 0.26
老年人 60 50 1.0 143.1 1927.3 0.01 0.16
), ArticleFig(id=1167158513362023141, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 6, caption=

Detection results of quinolones

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 检测
数量		 检出
数量		 检出率/% 残留范围
/(μg/kg)		 平均残留含量
/(μg/kg)		 不合格
数量		 不合格率
/%		 总体
不合格数量		 总体不合格率
/%
恩诺沙星 77 34 44.2 1.74~5585.00 245.10 14 18.2 14 18.2
氧氟沙星 77 2 2.6 36.30~65.60 1.32 2 2.6
培氟沙星 77 未检出 / / / / / / /
诺氟沙星 77 未检出 / / / / / / /
), ArticleFig(id=1167158513475269351, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表6, caption=

喹诺酮类抗生素的检出结果

, figureFileSmall=null, figureFileBig=null, tableContent=
目标化合物 检测
数量		 检出
数量		 检出率/% 残留范围
/(μg/kg)		 平均残留含量
/(μg/kg)		 不合格
数量		 不合格率
/%		 总体
不合格数量		 总体不合格率
/%
恩诺沙星 77 34 44.2 1.74~5585.00 245.10 14 18.2 14 18.2
氧氟沙星 77 2 2.6 36.30~65.60 1.32 2 2.6
培氟沙星 77 未检出 / / / / / / /
诺氟沙星 77 未检出 / / / / / / /
), ArticleFig(id=1167158513592709866, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 7, caption=

Detection results of quinolones in different species

, figureFileSmall=null, figureFileBig=null, tableContent=
品种 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
草鱼 15 2 13.3 3.79~30.60 2.30 0 0.0
黄颡鱼 12 11, 2* 91.7 6.82~1014.00, 36.30~65.60* 279.10, 8.50* 6 50.0
鲫鱼 12 4 33.3 6.94~679.00 59.10 1 8.3
鲈鱼 7 0 0.0 0 0 0 0.0
泥鳅 8 8 100.0 2.74~5585.00 1717.10 6 75.0
翘嘴鲌 3 0 0.0 0 0 0 0.0
鳝鱼 6 3 50.0 1.74~874.00 145.90 1 16.7
鳙鱼 10 4 40.0 7.43~54.90 58.20 0 0.0
鳊鱼 4 3 75.0 14.90~40.20 18.80 0 0.0
), ArticleFig(id=1167158513684984556, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表7, caption=

不同品种中喹诺酮的检出结果

, figureFileSmall=null, figureFileBig=null, tableContent=
品种 检测数量 检出数量 检出率/% 残留范围/(μg/kg) 平均残留含量/(μg/kg) 不合格数量 不合格率/%
草鱼 15 2 13.3 3.79~30.60 2.30 0 0.0
黄颡鱼 12 11, 2* 91.7 6.82~1014.00, 36.30~65.60* 279.10, 8.50* 6 50.0
鲫鱼 12 4 33.3 6.94~679.00 59.10 1 8.3
鲈鱼 7 0 0.0 0 0 0 0.0
泥鳅 8 8 100.0 2.74~5585.00 1717.10 6 75.0
翘嘴鲌 3 0 0.0 0 0 0 0.0
鳝鱼 6 3 50.0 1.74~874.00 145.90 1 16.7
鳙鱼 10 4 40.0 7.43~54.90 58.20 0 0.0
鳊鱼 4 3 75.0 14.90~40.20 18.80 0 0.0
), ArticleFig(id=1167158513781453551, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=EN, label=Table 8, caption=

Dietary risk assessment of quinolones

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物名称 人群 体重/kg 摄入量/(g/d) ADI
/[μg/(kg·bw)]		 平均残留含量/(μg/kg) RQ/%
氧氟沙星 儿童 20 40 5.0 1.32 0.05
成人 60 80 0.04
老年人 60 50 0.02
恩诺沙星 儿童 20 40 6.2 245.10 7.91
成人 60 80 5.27
老年人 60 50 3.29
), ArticleFig(id=1167158513894699761, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151881496466960840, language=CN, label=表8, caption=

喹诺酮的膳食风险评估

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物名称 人群 体重/kg 摄入量/(g/d) ADI
/[μg/(kg·bw)]		 平均残留含量/(μg/kg) RQ/%
氧氟沙星 儿童 20 40 5.0 1.32 0.05
成人 60 80 0.04
老年人 60 50 0.02
恩诺沙星 儿童 20 40 6.2 245.10 7.91
成人 60 80 5.27
老年人 60 50 3.29
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淡水鱼中渔用麻醉剂与喹诺酮类抗生素残留含量测定及膳食暴露风险评估
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李文博 , 谢柏艳 *
食品安全质量检测学报 | 专题：水产品加工与质量安全 2025,16(10): 126-133
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食品安全质量检测学报 | 专题：水产品加工与质量安全 2025, 16(10): 126-133
淡水鱼中渔用麻醉剂与喹诺酮类抗生素残留含量测定及膳食暴露风险评估
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李文博 , 谢柏艳*
作者信息
  • 武汉药品医疗器械检验所, 武汉 430075

    • 李文博(1989—), 男, 硕士, 主管药师, 主要研究方向为食品质量安全研究。E-mail:

通讯作者:

* 谢柏艳(1982—), 女, 硕士, 主管药师, 主要研究方向食品质量安全研究。E-mail:
Determination of fish sedatives and quinolones residues in freshwater fish and assessment of dietary exposure risk
Wen-Bo LI , Bai-Yan XIE*
Affiliations
  • Wuhan Institute for Drug and Medical Device Control, Wuhan 430075, China
出版时间: 2025-05-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250302001
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摘要
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目的 测定市售淡水鱼中渔用麻醉剂和喹诺酮类抗生素的残留含量并评估其膳食暴露风险。方法 在武汉市8个行政区域中共收集77批淡水鱼, 采用高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分别测定渔用麻醉剂(MS-222、苯佐卡因、丁香酚)及喹诺酮类抗生素(恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星)的含量, 用点评估法分析各化合物的膳食暴露风险。结果 所有样品中均未检出MS-222和苯佐卡因, 检出丁香酚48批次, 含量范围为2.59~1927.30 μg/kg, 不合格率为29.8%, 各年龄段人群膳食暴露风险值均小于0.4%, 膳食风险低。所有样品均未检出培氟沙星和诺氟沙星, 检出恩诺沙星34批, 含量范围为1.74~5585.00 μg/kg, 氧氟沙星2批, 含量范围为36.30~65.60 μg/kg, 总体不合格率为18.2%, 各年龄段人群的膳食暴露风险均小于8.00%。按品种分析, 泥鳅和黄颡鱼中恩诺沙星的含量范围分别为: 2.74~5585.00 μg/kg和6.82~1014.00 μg/kg, 膳食风险分别为: 55.4%和9.0%。结论 该地区使用的渔用麻醉剂为丁香酚, 其特点是检出率高和残留量大, 需要制定规范性文件指导使用。恩诺沙星作为主要的喹诺酮类抗生素药物在该地区使用, 有两个高风险品种: 泥鳅和黄颡鱼, 市场监管部门应重点关注这两个品种的监管。

渔用麻醉剂  /  喹诺酮类抗生素  /  残留含量  /  膳食暴露风险评估

Objective To determine the residual levels of fish sedatives and quinolones residues in commercially freshwater fish and evaluate their dietary exposure risk. Methods A total of 77 batches of freshwater fish were collected in 8 administrative regions of Wuhan City. High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used to determine the content of fishing anesthetics (MS-222, benzocaine, eugenol) and quinolone antibiotics (enrofloxacin, ciprofloxacin, ofloxacin, levofloxacin, levofloxacin, norfloxacin), and the dietary exposure risk of each compound was analyzed using a quantitative analysis method. Results MS-222 and benzocaine were not detected in all samples, and 48 batches of eugenol were detected with a content range of 2.59-1927.30 μg/kg, with a failure rate of 29.8%. The dietary exposure risk values for all age groups were less than 0.4%, indicating low dietary risk. All samples did not detect peofloxacin and norfloxacin. Enrofloxacin was detected in 34 batches with a content range of 1.74-5585.00 μg/kg, and ofloxacin was detected in 2 batches with a content range of 36.30-65.60 μg/kg, the overall failure rate was 18.2%, and the dietary exposure risk of all age groups was less than 8.00%. According to species analysis, the content range of enrofloxacin in loaches and yellow catfish was as follows: 2.74-5585.00 μg/kg and 6.82-1014.00 μg/kg, with dietary risks of 55.4% and 9.0%, respectively. Conclusion The fishery anesthetic used in this region is eugenol, which is characterized by high detection rate and large residual amount, and requires the development of normative documents to guide its use. Enrofloxacin, as the main quinolone antibiotic used in the region, has two high-risk species: Loach and yellow catfish. Market regulatory authorities should focus on the supervision of these two species.

fish sedatives  /  quinolones  /  residues  /  assessment of dietary exposure risk
李文博, 谢柏艳. 淡水鱼中渔用麻醉剂与喹诺酮类抗生素残留含量测定及膳食暴露风险评估. 食品安全质量检测学报, 2025 , 16 (10) : 126 -133 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250302001
Wen-Bo LI, Bai-Yan XIE. Determination of fish sedatives and quinolones residues in freshwater fish and assessment of dietary exposure risk[J]. Journal of Food Safety & Quality, 2025 , 16 (10) : 126 -133 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250302001
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0 引言
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鱼类产品因低脂、微量元素丰富, 且含有优质的蛋白质等特点受到广大消费者的喜爱[1-2]。国家农业农村部公布的数据显示, 2023年全国淡水鱼养殖产量达2771.59万t, 同比增长2.25%, 这表明消费者对淡水鱼的需求旺盛[3-4]。随着经济的发展, 消费者对淡水鱼的质量和新鲜度有了更高的要求。为了满足不同地区消费者的需求, 长途运输必不可少。但在长途运输过程中, 淡水鱼受应激胁迫、机体受伤感染和水质恶化等因素影响, 不仅引起存活率低的问题, 而且会使水产品质量降低[5-6]。针对此类问题, 国内外常用的方法是使用麻醉剂[7-9], 可降低淡水鱼的应激反应, 有效地提高了存活率。目前常用的渔用麻醉剂有丁香酚类、间氨基苯甲酸乙酯甲磺酸盐(MS-222)、苯佐卡因等。MS-222是美国食品药品监督管理局(Food and Drug Administration, FDA)批准的唯一可用于水产品中的麻醉剂, 具有见效快、麻醉时间短、麻醉持续长、复苏时间短和安全性高等特点[10-11]。苯佐卡因是MS-222的异构体, 被挪威批准用于水产品的麻醉。丁香酚作为渔用麻醉剂, 可以在日本、澳大利亚、智利和新西兰等国使用, 其具有低成本、高效和残留期短等特点[12-14], 日本规定丁香酚的最高残留限量(maximum residue limit, MRL)为0.05 mg/kg。我国目前还未批准可以合法使用的渔用麻醉剂, 市场上存在渔用麻醉剂滥用的情况。已有的研究表明, 我国市场上最常用的渔用麻醉剂为丁香油水门汀[15], 其中99.0%的成分为丁香酚。麻醉剂在使用时应严格遵守休药期[11], 例如MS-222休药期为21 d, 丁香酚的休药期为7 d, 但部分商贩为了尽快谋利, 存在休药期不足即上市的情况, 这会危害消费者的健康。
淡水鱼类在养殖、运输及出售过程中均存在高密度贮存的情况, 使其生存环境恶化, 导致疾病频发[16-17]。喹诺酮类药物与其他抗生素(四环素类、β-内酰胺类)相比具有广谱、强力、相对安全、价廉、副作用低的特性, 受到生产者和经营者的青睐[18-19]。但在喹诺酮类药物的实际使用中存在误用、滥用的情况, 不仅会使其在环境中残留, 还会使人体产生耐药性, 危害消费者健康。尤其是对于儿童, 可能会引起儿童关节及软组织的损伤, 临床上禁止18岁以下儿童使用喹诺酮类药物。
本研究以常见的淡水鱼类为研究对象, 采用高效液相色谱-串联质谱法(high performance liquid chromatography- tandem mass spectrometry, HPLC-MS/MS)测定淡水鱼类中渔用麻醉剂(MS-222、苯佐卡因、丁香酚)及喹诺酮类抗生素(恩诺沙星、环丙沙星、氧氟沙星、诺氟沙星)等, 并利用点评估法评估各风险因子的膳食暴露风险, 以期为淡水鱼的合理用药, 保障淡水鱼质量安全提供数据支持。
1 材料与方法
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1.1 样品的采集
本研究参考《湖北省食品安全监督抽检实施细则》(2024版)及GB/T 30891—2014《水产品抽样规范》的采样方法, 在武汉市8个行政区域的超市、农贸市场和生鲜店中共购买淡水鱼77批次, 每批次不少于3尾。品种分别为鳊鱼(4批)、草鱼(15批)、黄颡鱼(12批)、鲫鱼(12批)、鲈鱼(7批)、泥鳅(8批)、翘嘴鲌(3批)、鳝鱼(6批)、鳙鱼(10批)。样品购买完成后, 于4~8 ℃条件下, 8 h内运输至实验室, 取可食部分粉碎匀浆后于-20 ℃冷冻保存, 于10 d内完成检测。
1.2 试剂
无水硫酸镁、无水硫酸钠、氢氧化铵、二甲亚砜(分析纯, 国药集团化学试剂有限公司); 醋酸铵(色谱纯, 美国赛默飞公司); 甲醇、乙腈、甲酸(色谱纯, 德国Merck公司); C18 [50 μm, 纳谱分析技术(苏州)有限公司]; 恩诺沙星(批号G1116914, 纯度99.24%)(德国Dr.Ehrenstorfer公司); 诺氟沙星(批号23110051, 纯度99.6%)、环丙沙星(批号23050408, 纯度98.0%)、氘代环丙沙星(批号23110452, 100 μg/mL)(北京坛墨质检科技有限公司); 氧氟沙星(批号ALT086062-3, 纯度98.6%)(美国A ChemTek Inc公司); MS-222(批号D138315, 纯度93.7%)、氘代诺氟沙星(批号S166433, 100.3 μg/mL)、氘代恩诺沙星(批号S128791, 100 μg/mL)(天津阿尔塔科技有限公司); 培氟沙星(批号201402, 纯度71.3%)、丁香酚(批号202318, 纯度99.6%)、苯佐卡因(批号201602, 纯度99.9%)(中国食品药品检定研究院)。
1.3 仪器与设备
API4000三重四极杆液质联用仪(美国AB SCIEX公司); XS105电子天平(精度0.01 mg, 瑞士MEITLER TOLEDO公司); L-530台式低速离心机(湖南湘仪实验室仪器开发有限公司); JPCQ1028超声仪(武汉嘉鹏电子有限公司); InertSustain C18色谱柱(150 mm×2.1 mm, 5.0 μm, 日本岛津公司); CAPCELL C18色谱柱(150 mm×2.0 mm, 5.0 μm, 日本OSAKA SODA公司)。
1.4 实验方法
1.4.1 淡水鱼中喹诺酮类抗生素的测定方法
本研究按农业部1077号公告-1-2008《水产品中17种磺胺类及15种喹诺酮类药物残留量的测定》测定样品中的喹诺酮类抗生素。
1.4.2 淡水鱼中渔用麻醉剂的测定方法
本研究参考GB 31656.6—2021《水产品中丁香酚残留量的测定》和BJS 202110《水产品及相关用水中12种卡因类麻醉剂及其代谢物的测定》测定样品中的渔用麻醉剂。称取试样2.00 g至50 mL离心管中, 加入5 g无水硫酸钠, 加入10 mL乙腈, 涡旋1 min, 超声20 min, 3000 r/min离心10 min, 取上清液5.0 mL至净化管(含C18 100 mg, 无水硫酸镁500 mg)中, 涡旋5 min, 然后3000 r/min离心5 min, 取出上清液, 加入50 μL二甲亚砜, 40 ℃氮吹至近干, 加入1 mL 20%乙腈溶液复溶, 过0.45 μm滤膜, 供HPLC-MS/MS分析。
1.4.3 膳食暴露风险的评估方法
(1)膳食风险的计算方法
采用联合国粮农组织(United Nations Food and Agriculture Organization, FAO)/世界卫生组织(World Health Organization, WHO)推荐的《食品中化学物风险评估原则和方法》膳食风险评估方法中“点评估”法[20], 按照公式(1)分别计算渔用麻醉剂和喹诺酮类抗生素的膳食暴露风险。
RQ=(LP×C)/(bw×ADI)×100%
式中: RQ为膳食暴露风险(risk quotient); LP为居民日均消费量, g/d; C为样品中化学物质残留量, mg/kg; bw为平均体重, kg; ADI为每日允许摄入量(allowable daily intake), mg/(kg·bw)。
RQ越小风险越小, 当RQ≤100%时, 表示风险可以接受; 反之, 当RQ>100%时, 表示有不可接受的风险。
(2)相关参数的确定
国家体育总局于2022年发布的《第五次国民体质监测公报》[21]显示儿童(3~6岁)平均体重约为20 kg; 男、女成人(20~60岁)平均体重分别为70 kg和60 kg, 为了使风险评估更加严谨, 成人体重取60 kg; 老年人平均体重约为60 kg。《中国居民膳食指南(2022版)》[22]中推荐儿童(2~6岁)、成人(18~64岁)、老人(65岁以上)水产品最高食用量分别为280、525、350 g/周, 折算每天食用量为: 40、80、50 g/d。
1.5 数据处理
本研究采用Sciex-Analyst®1.5.2软件对数据进行定量计算, 利用Excel 2010进行数据分析和制图。
2 结果与分析
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2.1 方法学验证结果
取鲈鱼阴性样品作空白基质, 按1.4.1和1.4.2项下操作分别制备喹诺酮类及渔用麻醉剂的基质混合标准工作溶液、回收率溶液。结果显示两个方法的线性相关性良好, 相关系数(r)均不小于0.998, 检出限(limit of detection, LOD)、定量限(limit of quantification, LOQ)、回收率及相对标准偏差(relative standard deviation, RSD)满足本研究要求。喹诺酮类药物方法学验证结果见表1, 渔用麻醉剂方法学验证结果见表2。
2.2 渔用麻醉剂的检出结果及分析
丁香酚作为食品添加剂, GB 2760—2024《食品安全国家标准 食品添加剂使用标准》中规定其作为香料使用, 但要求附录B1不得添加香精香料, 鲜水产在名单之内。日本肯定列表中规定鱼类中丁香酚的限度为0.05 mg/kg, 故本研究将残留含量大于0.05 mg/kg的样品判定为不合格。对收集的77批次淡水鱼进行测定, 均未检出MS-222和苯佐卡因, 48批样品中检出丁香酚, 具体结果见表3。结果显示, 国内市场中渔用麻醉剂使用频率最高的是丁香酚, 这与林晨等[23]、周华等[24]的研究结果一致。相较于2015年国家水产品质量安全风险评估项目组评估水产品中丁香酚的检出率为10.6%, 2017年湖北省课题项目组的淡水产品中丁香酚的检出率为32.5%[25], 本研究中丁香酚的检出率为62.3%, 原因可能是本研究的样品收集时间为5至8月份, 地区气候炎热, 出于降低鱼类新陈代谢的目的, 大量使用丁香酚。王鹏等[26]的研究表明, 分别在春、夏两季采样, 夏季丁香酚的检出率要明显高于春季。另一方面可能是我国没有相应的规范指导渔用麻醉剂的使用, 没有制定丁香酚的限值, 在日常的监督抽检中也无该检验项目, 导致丁香酚在本地区有滥用的情况。相较于2015年和2017年的研究中丁香酚最高残留量分别为36.1 mg/kg和3.62 mg/kg, 本研究中最高残留量为1.93 mg/kg (1927.30 μg/kg), 呈下降趋势, 但仍是日本规定限度的39倍, 原因可能是经营者在使用丁香酚后, 未按照相关要求执行休药期, 日本规定鱼类在使用丁香酚后需休药7 d方可食用。检出率高和残留量大的特点均反映出丁香酚存在滥用的情况, 这提示相关部门应尽快制定渔用麻醉剂的指导性文件及最大限值, 规范市场行为。
按照种类不同, 统计分析各品种的丁香酚检出情况, 具体结果见表4。结果显示, 所有品种均检出丁香酚, 其中草鱼、黄颡鱼、鲫鱼、鳊鱼和翘嘴鲌的检出率均超过60%。不合格率较高的品种为草鱼和鳊鱼, 其平均残留量分别超标7倍和5倍。不同品种间检出率和不合格率存在差异的原因可能是不同品种间麻醉敏感性、耐低氧性、性情的不同。草鱼的检出和不合格均处于高位, 原因可能是草鱼体型较大、性情活泼, 在捕捞和转运过程中需要进入较深的麻醉状态, 否则会产生过大的应激反应。同为大型鱼类的鳙鱼, 因性情安静, 不合格率则较低。鳊鱼的耐低氧能力较差, 丁香酚可以显著降低耗氧量, 提高转运的成活率。
2.3 渔用麻醉剂的膳食暴露风险评估
FAO/WHO推荐丁香酚的ADI值为2.5 mg/(kg·bw), 欧洲食品安全局(European Food Safety Authority, EFSA)则规定丁香酚的ADI值为1.0 mg/(kg·bw)。本研究为了更加严谨地评估丁香酚的膳食风险, ADI值取EFSA的规定值1.0 mg/(kg·bw)。按公式(1)计算不同年龄段人群的膳食风险, 具体结果见表5。结果显示, 分别按平均残留量和最高残留量计算膳食暴露风险均远低于100%, 膳食风险较低, 目前处于相对安全的水平。但FDA的相关研究显示丁香酚对啮齿动物有可疑致癌性或潜在致癌性[27-28], 出于安全考虑其未将丁香酚作鱼类的麻醉剂。ADI值的确定是个动态研究的过程, 随着研究的深入, 会不断调整, 按目前的研究结果, 淡水鱼类中丁香酚的膳食风险可以接受, 但不排除将来修订后出现膳食风险的可能。针对国内常用丁香酚作为麻醉剂的情况, 相关部门应加强丁香酚在毒理学方面研究, 制定合理的限值, 以规避未来可能出现的风险。
2.4 喹诺酮类抗生素的检出结果及分析
77批次淡水鱼中均未检出诺氟沙星和培氟沙星, 检出恩诺沙星34批和氧氟沙星2批, 具体测定结果见表6。GB 31650—2019《食品安全国家标准 食品中兽药最大残留限量》规定恩诺沙星(以恩诺沙星和环丙沙星和计)在鱼中最大残留量为100 μg/kg, 《农业部公告第2292号》规定洛美沙星、培氟沙星、氧氟沙星、诺氟沙星等在鱼中不得使用。结果显示, 32批次样品中检出一种抗生素—恩诺沙星, 2批次样品中同时检出氧氟沙星和恩诺沙星。恩诺沙星的总体检出率为44.2%, 不合格率为18.2%。相关的研究显示, 贝亦江等[29]发现在流通环节恩诺沙星的检出率为51.3%, 不合格率为12.2%; 曹爱巧等[30]报道生产环节和流通环节淡水鱼中喹诺酮类抗生素检出率为33.4%, 不合格率为1.4%。研究结果提示, 本地区淡水鱼中喹诺酮类抗生素主要使用种类为恩诺沙星, 与其他地区结果一致。检出率与报道的流通环节检出率相近, 高于生产和流通环节总检出率, 龙举等[31]的研究中也提出了流通环节的检出率和不合格率是生产环节的5倍。本研究中恩诺沙星平均残留量超标2.5倍、最高残留量超标56倍, 不合格率相较于其他研究, 处于高位。
按照种类不同, 统计分析各品种中喹诺酮类抗生素的检出情况, 具体结果见表7。结果显示, 除鲈鱼和翘嘴鲌未检出, 其他品种中均检出喹诺酮类抗生素。检出不合格的品种有黄颡鱼、泥鳅、鳝鱼和鲫鱼, 均为体型较小的鱼类。尤其值得关注的是黄颡鱼和泥鳅, 其不合格率分别为50.0%和75.0%, 平均残留量分别超标2.8倍和17倍, 最高残留量超标10倍和56倍, 其中黄颡鱼中2批次检出禁止添加的氧氟沙星, 超标情况严重。小型鱼类中喹诺酮抗生素不合格率高的原因可能是生存密度过大, 易导致细菌性疾病暴发, 为了提高存活率, 超量使用喹诺酮抗生素。
2.5 喹诺酮类抗生素的膳食暴露风险评估
GB 31650—2019中推荐恩诺沙星、氧氟沙星的ADI值分别为6.2 μg/(kg·bw)、5.0 μg/(kg·bw), 按公式(1)计算不同年龄段人群的膳食风险, 具体结果见表8。结果显示, 按平均残留量计算膳食暴露风险, 氧氟沙星和恩诺沙星均小于100%, 食用风险较小。不同品种的淡水鱼中恩诺沙星平均残留量相差较大, 尤其是黄颡鱼和泥鳅无论是检出率还是不合格率均处于高位, 因此有必要对不同品种进行膳食风险的评估, 评估选择儿童的相关参数进行计算, 具体结果见图1。结果显示, 不同品种间按风险排序为: 泥鳅>黄颡鱼>鳝鱼>鲫鱼≈鳙鱼>鳊鱼>草鱼, 泥鳅的风险值已超过50%。湖北地区淡水资源丰富, 泥鳅是本地区人群喜食的鱼类, 摄入量可能会超过推荐摄入量, 造成膳食风险不可接受, 引起健康问题。造成泥鳅风险较高的原因可能是泥鳅是穴居动物, 喜欢在渔场底部的淤泥中生存, 而相关研究表明[32], 湖底淤泥中含有喹诺酮类抗生素, 从而造成其含量超标, 另外泥鳅在生产和流通环境的生存密度较大, 容易损伤, 使得经营者出现超量使用抗生素的情况。
3 结论与讨论
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本研究测定了武汉市不同区域的77批次淡水鱼中渔用麻醉剂和喹诺酮类抗生素的含量, 并进行了膳食风险评估。研究发现该地区使用的渔用麻醉剂种类为丁香酚, 检出率为62.3%, 按照日本规定的限度进行判定, 不合格率为29.8%, 相较于以往的研究, 丁香酚的使用频率呈上涨趋势, 说明该地区可能存在麻醉剂滥用的风险。进行膳食风险评估, RQ值远低于100%, 处于相对安全的水平。考虑到引起的原因可能是样品收集时间处于炎热气候, 下一步将对不同季节的样品进行评估。另有相关的研究指出, FDA不批准丁香酚在鱼类中使用的原因是丁香酚中含有甲基丁香酚, 甲基丁香酚具有致癌性, 针对目前国内将丁香酚作为最常用的渔用麻醉剂, 有必要进一步研究甲基丁香酚的残留量。77批样品中检出喹诺酮类抗生素的种类为恩诺沙星和氧氟沙星, 检出率分别为44.2%和2.6%。氧氟沙星阳性的样品中恩诺沙星同时超标, 不合格率为18.2%, 与以往流通环节的研究相比, 恩诺沙星的检出率相近, 不合格率较高。经膳食风险评估, 恩诺沙星的总体风险较低。但对各品种分析时发现泥鳅和黄颡鱼中恩诺沙星的残留量在检出率和不合格率上均明显高于其他品种, 且泥鳅的膳食风险超过50%, 可能会影响特殊人群如儿童、孕妇和泥鳅喜爱者的健康问题。
目前我国尚无针对渔用麻醉剂出台相关的标准指导, 未明确应使用哪种渔用麻醉剂并制定相应的最大残留量, 可能会造成渔用麻醉剂的使用混乱, 引起健康风险。本研究受限于收集数量不足, 可能导致喹诺酮类抗生素的不合格率估算偏高, 但可以一定程度上反映其在该地区淡水鱼类中的残留情况, 并筛选出泥鳅和黄颡鱼两个高风险品种, 对监管部门规范市场有一定参考意义。
基金
收起
  • 湖北省市场监督管理局科技计划项目(Hbscjg-KJ2022002)
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2025年第16卷第10期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250302001
  • 接收时间：2025-03-02
  • 首发时间：2025-07-15
  • 出版时间：2025-05-25
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  • 收稿日期：2025-03-02
基金
湖北省市场监督管理局科技计划项目(Hbscjg-KJ2022002)
作者信息
    武汉药品医疗器械检验所, 武汉 430075

通讯作者:

* 谢柏艳(1982—), 女, 硕士, 主管药师, 主要研究方向食品质量安全研究。E-mail:
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2种不同金属材料的力学参数
科
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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