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Article(id=1215670314474853076, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250410001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1744214400000, receivedDateStr=2025-04-10, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1767767989033, onlineDateStr=2026-01-07, pubDate=1753372800000, pubDateStr=2025-07-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1767767989033, onlineIssueDateStr=2026-01-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1767767989033, creator=13701087609, updateTime=1767767989033, updator=13701087609, issue=Issue{id=1215670311140381365, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='14', pageStart='1', pageEnd='326', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1767767988237, creator=13701087609, updateTime=1767970098618, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1216518023599538606, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1216518023599538607, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1215670311140381365, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=139, endPage=146, ext={EN=ArticleExt(id=1215670314810397413, articleId=1215670314474853076, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 50 kinds of antibiotic residues in dried sea cucumbers by multifunctional purification column with ultra performance liquid chromatography-tandem mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for simultaneous determination of 50 kinds of antibiotics in dried sea cucumbers by multifunctional purification column combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with 50% acetonitrile aqueous solution. After purification by multifunctional purification column, 50 kinds of antibiotics were separated using Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm) column with acetonitrile and 0.1% formic acid aqueous solution (include 5mmol/L ammonium acetate) for gradient elution. The mass spectrum was performed by electrospray positive ion mode scanning and multi-reaction monitoring acquisition, and quantified by external standard method. Results The results showed that 50 kinds of antibiotics exhibited good linearity in the range of 0.1-100.0 ng/mL, and the correlation coefficients were all greater than 0.99. The limit of detection ofthe method was 0.1-2.0 µg/kg, the limit of quantitation was 0.5-5.0 μg/kg. Recovery tests were carried out at 3 levels (1 times, 2 times, 10 times of the limit of quantitation) in the blank matrix, the average recoveries of the limit of detection were in the range of 54.83%-120.01%, and all the relative standard deviations (n=6) were 0.08%-9.15%. Conclusion This method has the technical advantages of simple operation process, excellent detection sensitivity, reliable precision, and good reproducibility, it can be applied to rapid screening and qualitative and quantitative detection of multiple antibiotics in dried sea cucumbers.

, correspAuthors=Liang-Liang QIAN, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Yan-Yan GONG, Liang-Liang QIAN), CN=ArticleExt(id=1215670315976413991, articleId=1215670314474853076, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=超高效液相色谱-串联质谱法结合多功能净化柱测定干海参中50种抗生素残留, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立多功能净化柱净化结合超高效液相色谱-串联质谱法同时检测干海参中50种抗生素的分析方法。方法 样品经50%乙腈水溶液提取, 多层复合净化柱净化, 采用Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm)色谱柱分离, 流动相为乙腈和0.1%甲酸水(含5 mmol/L乙酸铵), 进行梯度洗脱, 质谱采用电喷雾正离子模式扫描模式和多反应监测采集方式, 基质匹配外标法定量分析。结果 50种抗生素在0.1~100.0 ng/mL质量浓度范围内具有良好的线性关系, 相关系数均大于0.99, 方法检出限在0.1~2.0 μg/kg之间, 定量限在0.5~5.0 μg/kg之间。考察基质空白在(1倍、2倍、10倍定量限)3个不同浓度时加标实验, 样品加标回收率为54.83%∼120.01%, 相对标准偏差(n=6)为0.08%∼9.15%。结论 该方法具备操作流程简便、检测灵敏度优异、精密度可靠及重现性良好的技术优势, 适用于干海参中多种抗生素的快速筛查以及定性定量分析检测。

, correspAuthors=钱亮亮, authorNote=null, correspAuthorsNote=
*钱亮亮(1984—), 男, 正高级工程师, 主要研究方向为食品检测与质量安全控制。E-mail:
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宫艳艳(1983—), 女, 硕士, 高级工程师, 主要研究方向为食品检测与质量安全控制。E-mail:

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宫艳艳(1983—), 女, 硕士, 高级工程师, 主要研究方向为食品检测与质量安全控制。E-mail:

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Determination of macrolide antibiotics in the sediment based on dispersed solid-phase extraction coupled with ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Environmental Chemistry, 2022, 41(1): 231-240., articleTitle=Determination of macrolide antibiotics in the sediment based on dispersed solid-phase extraction coupled with ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry, refAbstract=null), Reference(id=1215670329121362558, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, doi=null, pmid=null, pmcid=null, year=2024, volume=46, issue=6, pageStart=99, pageEnd=106, url=null, language=null, rfNumber=[33], rfOrder=45, authorNames=李增明, 解玉龙, 马春光, journalName=化学试剂, refType=null, unstructuredReference=李增明, 解玉龙, 马春光. QuEChERS-超高效液相色谱-串联质谱法测定牦牛肉中多种抗生素残留[J]. 化学试剂, 2024, 46(6): 99-106., articleTitle=QuEChERS-超高效液相色谱-串联质谱法测定牦牛肉中多种抗生素残留, refAbstract=null), Reference(id=1215670329242997384, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, doi=null, pmid=null, pmcid=null, year=2024, volume=46, issue=6, pageStart=99, pageEnd=106, url=null, language=null, rfNumber=[33], rfOrder=46, authorNames=LI ZM, JIE YL, MA CG, journalName=Chemical Reagents, refType=null, unstructuredReference=LI ZM, JIE YL, MA CG. Determination of veterinary drug residues in yak meat by QuEChERS-ultra performance liquid chromatography- tandem mass spectrometry[J]. Chemical Reagents, 2024, 46(6): 99-106., articleTitle=Determination of veterinary drug residues in yak meat by QuEChERS-ultra performance liquid chromatography- tandem mass spectrometry, refAbstract=null)], funds=[Fund(id=1215670320493678648, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, awardId=NL2021047, language=CN, fundingSource=江苏省市场监督管理局技术能力提升项目(NL2021047), fundOrder=null, country=null), Fund(id=1215670320573370436, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, awardId=SF2331, language=CN, fundingSource=连云港市科技计划项目(SF2331), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1215670316270015287, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, xref=1, ext=[AuthorCompanyExt(id=1215670316290986810, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, companyId=1215670316270015287, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 Lianyungang Food and Drug Inspection and Testing Center, Lianyungang 222000, China), AuthorCompanyExt(id=1215670316299375419, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, companyId=1215670316270015287, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 连云港市食品药品检验检测中心, 连云港 222000)]), AuthorCompany(id=1215670316383261505, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, xref=2, ext=[AuthorCompanyExt(id=1215670316391650114, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, companyId=1215670316383261505, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Lianyungang Comprehensive Inspection and Testing Center for Quality and Technology, Lianyungang 222000, China), AuthorCompanyExt(id=1215670316395844419, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, companyId=1215670316383261505, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 连云港市质量技术综合检验检测中心, 连云港 222000)])], figs=[ArticleFig(id=1215670319143113668, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=EN, label=Fig.1, caption=Comparison of recovery rates between foamed and unfoamed sea cucumbers, figureFileSmall=fIyHjWyKKyDKYwLzw9pSyg==, figureFileBig=mJZSG4Kqu7c5A2W8tVeJqg==, tableContent=null), ArticleFig(id=1215670319235388365, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=CN, label=图1, caption=发泡与未发泡海参的回收率对比, figureFileSmall=fIyHjWyKKyDKYwLzw9pSyg==, figureFileBig=mJZSG4Kqu7c5A2W8tVeJqg==, tableContent=null), ArticleFig(id=1215670319449297889, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=EN, label=Fig.2, caption=Detection results of 3 positive samples, figureFileSmall=+nK1eJ8KwnHXkaglFn8ZsA==, figureFileBig=QU/fNSxVFN7iV7ex647aQg==, tableContent=null), ArticleFig(id=1215670319549961197, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=CN, label=图2, caption=3个阳性样本的检出结果, figureFileSmall=+nK1eJ8KwnHXkaglFn8ZsA==, figureFileBig=QU/fNSxVFN7iV7ex647aQg==, tableContent=null), ArticleFig(id=1215670319654818804, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=EN, label=Table 1, caption=

Table of elution gradient

, figureFileSmall=null, figureFileBig=null, tableContent=
时间/min A/% B/%
0 95 5
1.5 95 5
8.0 70 30
11.0 5 95
13.0 5 95
13.1 95 5
15.0 95 5
), ArticleFig(id=1215670319763870719, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=CN, label=表1, caption=

洗脱梯度表

, figureFileSmall=null, figureFileBig=null, tableContent=
时间/min A/% B/%
0 95 5
1.5 95 5
8.0 70 30
11.0 5 95
13.0 5 95
13.1 95 5
15.0 95 5
), ArticleFig(id=1215670319885504524, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=EN, label=Table 2, caption=

MS parameters

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 化合物 母离子
(m/z)		 子离子
(m/z)		 去簇电压
/V		 碰撞能量
/V		 序号 化合物 母离子
(m/z)		 子离子
(m/z)		 去簇电压
/V		 碰撞能量
/V
1 沙拉沙星 386.1 342.1 90 27 26 磺胺苯酰 277.1 156.0 60 20
386.1 299.1 90 36 277.1 108.0 60 33
2 司帕沙星 393.1 292.1 80 37 27 磺胺喹恶啉 301.1 156.1 80 25
393.1 349.1 80 29 301.1 108.0 80 35
3 洛美沙星 352.0 265.0 80 33 28 磺胺嘧啶 251.1 156.0 60 23
352.0 308.1 80 28 251.1 92.0 60 37
4 氟甲喹 262.1 244.1 77 23 29 磺胺二甲氧
嘧啶		 311.1 156.1 82 28
262.1 202.1 77 42 311.1 218.0 82 27
5 氧氟沙星 362.2 318.1 80 25 30 磺胺多辛 311.1 156.1 63 31
362.2 261.1 80 37 311.1 108.2 63 36
6 奥比沙星 396.0 352.0 80 26 31 磺胺甲基嘧啶 265.2 156.1 82 25
396.0 295.2 80 33 265.2 172.1 82 27
7 苯唑西林 402.0 160.0 60 18 32 磺胺甲恶唑 254.1 108.0 81 36
402.0 243.0 60 17 254.1 188.1 81 19
8 马波沙星 363.1 320.1 80 23 33 磺胺二甲嘧啶 279.1 186.1 67 23
363.1 72.0 80 46 279.1 156.0 67 27
9 诺氟沙星 320.1 276.1 80 26 34 磺胺甲氧哒嗪 281.0 156.0 80 23
320.1 233.1 80 35 281.0 126.1 80 28
10 环丙沙星 332.2 231.0 110 50 35 磺胺间甲氧
嘧啶		 281.1 156.0 62 24
332.2 288.1 110 26 281.1 126.1 62 31
11 双氟沙星 400.1 356.1 82 28 36 磺胺苯吡唑 315.0 156.0 90 27
400.1 299.1 82 41 315.0 108.0 90 40
12 达诺沙星 358.0 340.0 65 30 37 磺胺噻唑 256.0 156.0 82 22
358.0 314.0 65 25 256.0 108.0 82 32
13 依诺沙星 321.0 303.0 60 24 38 磺胺异恶唑 268.1 156.1 69 22
321.0 234.0 60 30 268.1 113.2 69 25
14 恩诺沙星 360.1 316.1 80 28 39 磺胺醋酰 215.0 156.0 82 17
360.1 245.1 80 36 215.0 108.0 82 29
15 氟罗沙星 370.0 326.1 80 27 40 甲氧苄啶 291.1 230.1 83 33
370.0 269.2 80 35 291.1 123.1 83 34
16 螺旋霉素 843.3 142.2 60 48 41 头孢唑林 454.8 323.0 70 15
843.3 174.2 60 50 454.8 155.8 70 21
17 罗红霉素 837.6 679.5 50 31 42 氨苄西林 350.3 192.1 55 23
837.6 158.1 50 36 350.3 106.1 55 26
18 林可霉素 407.3 126.1 30 32 43 阿莫西林 366.2 349.1 47 13
407.3 359.2 30 27 366.2 114.1 47 30
19 红霉素 734.5 576.4 30 28 44 头孢吡肟 481.0 395.9 37 17
734.5 158.0 30 36 481.0 124.9 37 65
20 克林霉素 425.3 126.1 50 34 45 替米考星 869.5 696.5 100 50
425.3 377.1 50 27 869.5 174.2 100 55
21 克拉霉素 748.5 590.4 40 28 46 泰乐菌素 916.6 174.0 151 47
748.5 158.0 40 40 916.6 772.5 151 43
22 多西环素 445.0 428.1 80 26 47 氯霉素 321.0 152.1 -75 -24
445.0 154.1 80 36 321.0 256.9 -75 -17
23 金霉素 479.1 462.0 100 25 48 氟苯尼考 356.0 119.0 -80 -23
479.1 444.0 100 28 356.0 184.9 -80 -16
24 地美环素 465.0 448.0 81 24 49 氟苯尼考胺 248.2 230.1 50 16
465.0 430.0 81 32 248.2 130.1 50 30
25 四环素 445.1 410.2 80 26 50 甲砜霉素 353.9 289.9 -75 -18
445.1 427.1 80 18 353.9 184.9 -75 -28
), ArticleFig(id=1215670319986167831, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=CN, label=表2, caption=

质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 化合物 母离子
(m/z)		 子离子
(m/z)		 去簇电压
/V		 碰撞能量
/V		 序号 化合物 母离子
(m/z)		 子离子
(m/z)		 去簇电压
/V		 碰撞能量
/V
1 沙拉沙星 386.1 342.1 90 27 26 磺胺苯酰 277.1 156.0 60 20
386.1 299.1 90 36 277.1 108.0 60 33
2 司帕沙星 393.1 292.1 80 37 27 磺胺喹恶啉 301.1 156.1 80 25
393.1 349.1 80 29 301.1 108.0 80 35
3 洛美沙星 352.0 265.0 80 33 28 磺胺嘧啶 251.1 156.0 60 23
352.0 308.1 80 28 251.1 92.0 60 37
4 氟甲喹 262.1 244.1 77 23 29 磺胺二甲氧
嘧啶		 311.1 156.1 82 28
262.1 202.1 77 42 311.1 218.0 82 27
5 氧氟沙星 362.2 318.1 80 25 30 磺胺多辛 311.1 156.1 63 31
362.2 261.1 80 37 311.1 108.2 63 36
6 奥比沙星 396.0 352.0 80 26 31 磺胺甲基嘧啶 265.2 156.1 82 25
396.0 295.2 80 33 265.2 172.1 82 27
7 苯唑西林 402.0 160.0 60 18 32 磺胺甲恶唑 254.1 108.0 81 36
402.0 243.0 60 17 254.1 188.1 81 19
8 马波沙星 363.1 320.1 80 23 33 磺胺二甲嘧啶 279.1 186.1 67 23
363.1 72.0 80 46 279.1 156.0 67 27
9 诺氟沙星 320.1 276.1 80 26 34 磺胺甲氧哒嗪 281.0 156.0 80 23
320.1 233.1 80 35 281.0 126.1 80 28
10 环丙沙星 332.2 231.0 110 50 35 磺胺间甲氧
嘧啶		 281.1 156.0 62 24
332.2 288.1 110 26 281.1 126.1 62 31
11 双氟沙星 400.1 356.1 82 28 36 磺胺苯吡唑 315.0 156.0 90 27
400.1 299.1 82 41 315.0 108.0 90 40
12 达诺沙星 358.0 340.0 65 30 37 磺胺噻唑 256.0 156.0 82 22
358.0 314.0 65 25 256.0 108.0 82 32
13 依诺沙星 321.0 303.0 60 24 38 磺胺异恶唑 268.1 156.1 69 22
321.0 234.0 60 30 268.1 113.2 69 25
14 恩诺沙星 360.1 316.1 80 28 39 磺胺醋酰 215.0 156.0 82 17
360.1 245.1 80 36 215.0 108.0 82 29
15 氟罗沙星 370.0 326.1 80 27 40 甲氧苄啶 291.1 230.1 83 33
370.0 269.2 80 35 291.1 123.1 83 34
16 螺旋霉素 843.3 142.2 60 48 41 头孢唑林 454.8 323.0 70 15
843.3 174.2 60 50 454.8 155.8 70 21
17 罗红霉素 837.6 679.5 50 31 42 氨苄西林 350.3 192.1 55 23
837.6 158.1 50 36 350.3 106.1 55 26
18 林可霉素 407.3 126.1 30 32 43 阿莫西林 366.2 349.1 47 13
407.3 359.2 30 27 366.2 114.1 47 30
19 红霉素 734.5 576.4 30 28 44 头孢吡肟 481.0 395.9 37 17
734.5 158.0 30 36 481.0 124.9 37 65
20 克林霉素 425.3 126.1 50 34 45 替米考星 869.5 696.5 100 50
425.3 377.1 50 27 869.5 174.2 100 55
21 克拉霉素 748.5 590.4 40 28 46 泰乐菌素 916.6 174.0 151 47
748.5 158.0 40 40 916.6 772.5 151 43
22 多西环素 445.0 428.1 80 26 47 氯霉素 321.0 152.1 -75 -24
445.0 154.1 80 36 321.0 256.9 -75 -17
23 金霉素 479.1 462.0 100 25 48 氟苯尼考 356.0 119.0 -80 -23
479.1 444.0 100 28 356.0 184.9 -80 -16
24 地美环素 465.0 448.0 81 24 49 氟苯尼考胺 248.2 230.1 50 16
465.0 430.0 81 32 248.2 130.1 50 30
25 四环素 445.1 410.2 80 26 50 甲砜霉素 353.9 289.9 -75 -18
445.1 427.1 80 18 353.9 184.9 -75 -28
), ArticleFig(id=1215670320099414046, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=EN, label=Table 3, caption=

Linear equation, limit of detection, limit of quantitation, matrix spiked recovery rate and precision

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 化合物 线性方程 检出限/(μg/kg) 定量限/(μg/kg) 加标1
回收率/%		 加标2
回收率/%		 加标3
回收率/%		 RSDs/%
(n=6)
1 沙拉沙星 Y=1.38249e5X+1425.29323 (r=0.9985) 0.5 1.0 86.41 86.68 86.21 3.27
2 司帕沙星 Y=1.3256e6X+1.3451e5 (r=0.9976) 0.5 1.0 88.58 87.49 89.25 6.33
3 洛美沙星 Y=1.9265e5X+4505.9770 (r=0.9961) 0.5 1.0 98.82 99.09 98.62 4.27
4 氟甲喹 Y=3.6184e7X+2.622e6 (r=0.9992) 0.5 1.0 88.83 87.28 89.06 1.19
5 氧氟沙星 Y=1.42345e6X-3961.78390 (r=0.9986) 0.5 1.0 86.90 85.35 87.13 5.21
6 奥比沙星 Y=1.349e6X+1776.475 (r=0.9995) 0.5 1.0 88.53 87.89 88.76 2.11
7 苯唑西林 Y=4.376e4X+2244.5604 (r=0.9987) 0.5 1.0 83.20 83.02 82.56 1.48
8 马波沙星 Y=6.3708e5X+3571.921 (r=0.9962) 0.5 1.0 84.91 83.36 84.27 3.54
9 诺氟沙星 Y=1.1762e5X+3998.1210 (r=0.9990) 0.5 1.0 120.21 119.82 120.01 6.16
10 环丙沙星 Y=2.2526e5X+1755.63541 (r=0.9962) 0.5 1.0 97.61 96.06 96.97 0.59
11 双氟沙星 Y=1.1965e6X+1.6234e5 (r=0.9985) 0.5 1.0 95.89 95.71 96.12 1.36
12 达诺沙星 Y=1.23628e5X+1312.9332 (r=0.9988) 0.5 1.0 97.09 96.45 96.45 2.35
13 依诺沙星 Y=1.4489e5X+1253.6954 (r=0.9970) 0.5 1.0 92.65 91.56 92.45 4.42
14 恩诺沙星 Y=1.71045e6X+2.72672e4 (r=0.9982) 0.5 1.0 86.20 85.56 86.87 0.97
15 氟罗沙星 Y=1.28433e6X+96743.4996 (r=0.9991) 0.5 1.0 86.17 86.44 85.53 3.38
16 螺旋霉素 Y=1523.923X-1423.07734 (r=0.9967) 0.5 1.0 83.60 82.05 83.83 4.11
17 罗红霉素 Y=1.4534e6X-2242.4123 (r=0.9997) 0.5 1.0 94.39 93.30 94.62 8.16
18 林可霉素 Y=5.2196e6X-4.9476e5 (r=0.9987) 0.5 1.0 73.98 72.43 74.21 3.67
19 红霉素 Y=1.7143e6X+4.3767e5 (r=0.9975) 0.5 1.0 85.42 85.24 85.22 1.28
20 克林霉素 Y=3.29365e6X-2034.078 (r=0.9983) 0.5 1.0 80.93 80.75 80.29 8.83
21 克拉霉素 Y=1.5965e6X+2.9815e4 (r=0.9979) 0.5 1.0 75.37 76.92 75.17 6.06
22 多西环素 Y=1.8131e5X+2.42483e5 (r=0.9975) 1.0 2.0 74.81 75.90 74.61 4.23
23 金霉素 Y=5.43724e4X-7464.4185 (r=0.9968) 1.0 2.0 83.36 83.18 84.03 7.17
24 地美环素 Y=2.26243e4X+6675.4653 (r=0.9968) 1.0 2.0 79.90 78.35 80.13 6.25
25 四环素 Y=4.7006e4X+3.5766e4 (r=0.9962) 1.0 2.0 75.17 76.72 75.40 1.02
26 磺胺苯酰 Y=1585.4366X+1253.1456 (r=0.9980) 0.5 1.0 92.45 92.27 93.12 7.15
27 磺胺喹恶啉 Y=1076.6614X+1220.3841 (r=0.9977) 0.5 1.0 95.76 94.67 95.99 4.30
28 磺胺嘧啶 Y=1910.0965X+9326.0575 (r=0.9976) 0.5 1.0 97.62 96.53 98.29 2.51
29 磺胺二甲氧嘧啶 Y=5.6122e6X-2.31065e4 (r=0.9952) 0.5 1.0 94.67 94.94 95.34 6.24
30 磺胺多辛 Y=2.1405e6X+2.6237e4 (r=0.9968) 0.5 1.0 83.34 83.61 82.70 2.19
31 磺胺甲基嘧啶 Y=18264.4476X+2891.0276 (r=0.9980) 0.5 1.0 113.86 113.68 113.66 8.32
32 磺胺甲恶唑 Y=2.9452e4X+1413.8384 (r=0.9990) 0.5 1.0 112.07 111.89 112.30 4.66
33 磺胺二甲嘧啶 Y=2.3013e4X+802.6794 (r=0.9969) 0.5 1.0 94.58 93.49 93.94 1.50
34 磺胺甲氧哒嗪 Y=2.8451e6X+1461.0124 (r=0.9998) 0.5 1.0 97.97 96.42 97.77 0.67
35 磺胺间甲氧嘧啶 Y=2.9843e6X-2.1569e4 (r=0.9986) 0.5 1.0 81.47 81.65 81.27 1.72
36 磺胺苯吡唑 Y=1167.7813X+2642.2432 (r=0.9968) 0.5 1.0 92.38 92.65 92.61 3.36
37 磺胺噻唑 Y=2.3633e4X-593.0573 (r=0.9955) 0.5 1.0 108.72 108.54 109.39 7.26
38 磺胺异恶唑 Y=1168.9629X+1004.1348 (r=0.9960) 0.5 1.0 98.16 99.71 97.96 3.99
39 磺胺醋酰 Y=2542.6352X+657.1304 (r=0.9985) 0.5 1.0 89.53 90.17 90.20 9.15
40 甲氧苄啶 Y=5.834e4X+78.5302 (r=0.9970) 0.5 1.0 83.09 81.54 83.76 6.31
41 头孢唑林 Y=1620.2827X+655.0692 (r=0.9970) 2.0 5.0 69.70 69.52 70.37 4.19
42 氨苄西林 Y=2211.7653X+405.1209 (r=0.9994) 2.0 5.0 54.83 54.65 55.06 6.83
43 阿莫西林 Y=2531.7620X+143.1782 (r=0.9968) 2.0 5.0 60.74 60.56 60.54 7.91
44 头孢吡肟 Y=1333.1642X-206.8028 (r=0.9979) 2.0 5.0 67.87 67.69 68.10 5.44
45 替米考星 Y=2.6914e5X+939.0586 (r=0.9978) 1.0 2.0 94.16 94.80 94.39 0.08
46 泰乐菌素 Y=1.8246e6X+1285.8467 (r=0.9991) 1.0 2.0 99.42 98.78 100.09 1.13
47 氯霉素 Y=5579.5760X+114.2512 (r=0.9976) 0.1 0.5 91.18 90.54 90.54 2.46
48 氟苯尼考 Y=5599.432X+176.912 (r=0.9976) 0.5 1.0 89.17 90.72 89.84 5.58
49 氟苯尼考胺 Y=3474.2335X+508.1043 (r=0.9980) 0.5 1.0 86.17 85.53 86.84 4.82
50 甲砜霉素 Y=156.289X+1075.152 (r=0.9995) 0.5 1.0 75.71 75.53 75.51 2.63
), ArticleFig(id=1215670320225243177, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1215670314474853076, language=CN, label=表3, caption=

线性方程、检出限、定量限、基质加标回收率和精密度

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 化合物 线性方程 检出限/(μg/kg) 定量限/(μg/kg) 加标1
回收率/%		 加标2
回收率/%		 加标3
回收率/%		 RSDs/%
(n=6)
1 沙拉沙星 Y=1.38249e5X+1425.29323 (r=0.9985) 0.5 1.0 86.41 86.68 86.21 3.27
2 司帕沙星 Y=1.3256e6X+1.3451e5 (r=0.9976) 0.5 1.0 88.58 87.49 89.25 6.33
3 洛美沙星 Y=1.9265e5X+4505.9770 (r=0.9961) 0.5 1.0 98.82 99.09 98.62 4.27
4 氟甲喹 Y=3.6184e7X+2.622e6 (r=0.9992) 0.5 1.0 88.83 87.28 89.06 1.19
5 氧氟沙星 Y=1.42345e6X-3961.78390 (r=0.9986) 0.5 1.0 86.90 85.35 87.13 5.21
6 奥比沙星 Y=1.349e6X+1776.475 (r=0.9995) 0.5 1.0 88.53 87.89 88.76 2.11
7 苯唑西林 Y=4.376e4X+2244.5604 (r=0.9987) 0.5 1.0 83.20 83.02 82.56 1.48
8 马波沙星 Y=6.3708e5X+3571.921 (r=0.9962) 0.5 1.0 84.91 83.36 84.27 3.54
9 诺氟沙星 Y=1.1762e5X+3998.1210 (r=0.9990) 0.5 1.0 120.21 119.82 120.01 6.16
10 环丙沙星 Y=2.2526e5X+1755.63541 (r=0.9962) 0.5 1.0 97.61 96.06 96.97 0.59
11 双氟沙星 Y=1.1965e6X+1.6234e5 (r=0.9985) 0.5 1.0 95.89 95.71 96.12 1.36
12 达诺沙星 Y=1.23628e5X+1312.9332 (r=0.9988) 0.5 1.0 97.09 96.45 96.45 2.35
13 依诺沙星 Y=1.4489e5X+1253.6954 (r=0.9970) 0.5 1.0 92.65 91.56 92.45 4.42
14 恩诺沙星 Y=1.71045e6X+2.72672e4 (r=0.9982) 0.5 1.0 86.20 85.56 86.87 0.97
15 氟罗沙星 Y=1.28433e6X+96743.4996 (r=0.9991) 0.5 1.0 86.17 86.44 85.53 3.38
16 螺旋霉素 Y=1523.923X-1423.07734 (r=0.9967) 0.5 1.0 83.60 82.05 83.83 4.11
17 罗红霉素 Y=1.4534e6X-2242.4123 (r=0.9997) 0.5 1.0 94.39 93.30 94.62 8.16
18 林可霉素 Y=5.2196e6X-4.9476e5 (r=0.9987) 0.5 1.0 73.98 72.43 74.21 3.67
19 红霉素 Y=1.7143e6X+4.3767e5 (r=0.9975) 0.5 1.0 85.42 85.24 85.22 1.28
20 克林霉素 Y=3.29365e6X-2034.078 (r=0.9983) 0.5 1.0 80.93 80.75 80.29 8.83
21 克拉霉素 Y=1.5965e6X+2.9815e4 (r=0.9979) 0.5 1.0 75.37 76.92 75.17 6.06
22 多西环素 Y=1.8131e5X+2.42483e5 (r=0.9975) 1.0 2.0 74.81 75.90 74.61 4.23
23 金霉素 Y=5.43724e4X-7464.4185 (r=0.9968) 1.0 2.0 83.36 83.18 84.03 7.17
24 地美环素 Y=2.26243e4X+6675.4653 (r=0.9968) 1.0 2.0 79.90 78.35 80.13 6.25
25 四环素 Y=4.7006e4X+3.5766e4 (r=0.9962) 1.0 2.0 75.17 76.72 75.40 1.02
26 磺胺苯酰 Y=1585.4366X+1253.1456 (r=0.9980) 0.5 1.0 92.45 92.27 93.12 7.15
27 磺胺喹恶啉 Y=1076.6614X+1220.3841 (r=0.9977) 0.5 1.0 95.76 94.67 95.99 4.30
28 磺胺嘧啶 Y=1910.0965X+9326.0575 (r=0.9976) 0.5 1.0 97.62 96.53 98.29 2.51
29 磺胺二甲氧嘧啶 Y=5.6122e6X-2.31065e4 (r=0.9952) 0.5 1.0 94.67 94.94 95.34 6.24
30 磺胺多辛 Y=2.1405e6X+2.6237e4 (r=0.9968) 0.5 1.0 83.34 83.61 82.70 2.19
31 磺胺甲基嘧啶 Y=18264.4476X+2891.0276 (r=0.9980) 0.5 1.0 113.86 113.68 113.66 8.32
32 磺胺甲恶唑 Y=2.9452e4X+1413.8384 (r=0.9990) 0.5 1.0 112.07 111.89 112.30 4.66
33 磺胺二甲嘧啶 Y=2.3013e4X+802.6794 (r=0.9969) 0.5 1.0 94.58 93.49 93.94 1.50
34 磺胺甲氧哒嗪 Y=2.8451e6X+1461.0124 (r=0.9998) 0.5 1.0 97.97 96.42 97.77 0.67
35 磺胺间甲氧嘧啶 Y=2.9843e6X-2.1569e4 (r=0.9986) 0.5 1.0 81.47 81.65 81.27 1.72
36 磺胺苯吡唑 Y=1167.7813X+2642.2432 (r=0.9968) 0.5 1.0 92.38 92.65 92.61 3.36
37 磺胺噻唑 Y=2.3633e4X-593.0573 (r=0.9955) 0.5 1.0 108.72 108.54 109.39 7.26
38 磺胺异恶唑 Y=1168.9629X+1004.1348 (r=0.9960) 0.5 1.0 98.16 99.71 97.96 3.99
39 磺胺醋酰 Y=2542.6352X+657.1304 (r=0.9985) 0.5 1.0 89.53 90.17 90.20 9.15
40 甲氧苄啶 Y=5.834e4X+78.5302 (r=0.9970) 0.5 1.0 83.09 81.54 83.76 6.31
41 头孢唑林 Y=1620.2827X+655.0692 (r=0.9970) 2.0 5.0 69.70 69.52 70.37 4.19
42 氨苄西林 Y=2211.7653X+405.1209 (r=0.9994) 2.0 5.0 54.83 54.65 55.06 6.83
43 阿莫西林 Y=2531.7620X+143.1782 (r=0.9968) 2.0 5.0 60.74 60.56 60.54 7.91
44 头孢吡肟 Y=1333.1642X-206.8028 (r=0.9979) 2.0 5.0 67.87 67.69 68.10 5.44
45 替米考星 Y=2.6914e5X+939.0586 (r=0.9978) 1.0 2.0 94.16 94.80 94.39 0.08
46 泰乐菌素 Y=1.8246e6X+1285.8467 (r=0.9991) 1.0 2.0 99.42 98.78 100.09 1.13
47 氯霉素 Y=5579.5760X+114.2512 (r=0.9976) 0.1 0.5 91.18 90.54 90.54 2.46
48 氟苯尼考 Y=5599.432X+176.912 (r=0.9976) 0.5 1.0 89.17 90.72 89.84 5.58
49 氟苯尼考胺 Y=3474.2335X+508.1043 (r=0.9980) 0.5 1.0 86.17 85.53 86.84 4.82
50 甲砜霉素 Y=156.289X+1075.152 (r=0.9995) 0.5 1.0 75.71 75.53 75.51 2.63
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超高效液相色谱-串联质谱法结合多功能净化柱测定干海参中50种抗生素残留
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宫艳艳 1 , 钱亮亮 2, *
食品安全质量检测学报 | 食品分析与检测 2025,16(14): 139-146
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食品安全质量检测学报 | 食品分析与检测 2025, 16(14): 139-146
超高效液相色谱-串联质谱法结合多功能净化柱测定干海参中50种抗生素残留
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宫艳艳1 , 钱亮亮2, *
作者信息
  • 1 连云港市食品药品检验检测中心, 连云港 222000
  • 2 连云港市质量技术综合检验检测中心, 连云港 222000

    • 宫艳艳(1983—), 女, 硕士, 高级工程师, 主要研究方向为食品检测与质量安全控制。E-mail:

通讯作者:

*钱亮亮(1984—), 男, 正高级工程师, 主要研究方向为食品检测与质量安全控制。E-mail:
Determination of 50 kinds of antibiotic residues in dried sea cucumbers by multifunctional purification column with ultra performance liquid chromatography-tandem mass spectrometry
Yan-Yan GONG1 , Liang-Liang QIAN2, *
Affiliations
  • 1 Lianyungang Food and Drug Inspection and Testing Center, Lianyungang 222000, China
  • 2 Lianyungang Comprehensive Inspection and Testing Center for Quality and Technology, Lianyungang 222000, China
出版时间: 2025-07-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250410001
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摘要
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目的 建立多功能净化柱净化结合超高效液相色谱-串联质谱法同时检测干海参中50种抗生素的分析方法。方法 样品经50%乙腈水溶液提取, 多层复合净化柱净化, 采用Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm)色谱柱分离, 流动相为乙腈和0.1%甲酸水(含5 mmol/L乙酸铵), 进行梯度洗脱, 质谱采用电喷雾正离子模式扫描模式和多反应监测采集方式, 基质匹配外标法定量分析。结果 50种抗生素在0.1~100.0 ng/mL质量浓度范围内具有良好的线性关系, 相关系数均大于0.99, 方法检出限在0.1~2.0 μg/kg之间, 定量限在0.5~5.0 μg/kg之间。考察基质空白在(1倍、2倍、10倍定量限)3个不同浓度时加标实验, 样品加标回收率为54.83%∼120.01%, 相对标准偏差(n=6)为0.08%∼9.15%。结论 该方法具备操作流程简便、检测灵敏度优异、精密度可靠及重现性良好的技术优势, 适用于干海参中多种抗生素的快速筛查以及定性定量分析检测。

多功能净化柱  /  超高效液相色谱-串联质谱法  /  干海参  /  抗生素残留

Objective To establish a method for simultaneous determination of 50 kinds of antibiotics in dried sea cucumbers by multifunctional purification column combined with ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with 50% acetonitrile aqueous solution. After purification by multifunctional purification column, 50 kinds of antibiotics were separated using Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm) column with acetonitrile and 0.1% formic acid aqueous solution (include 5mmol/L ammonium acetate) for gradient elution. The mass spectrum was performed by electrospray positive ion mode scanning and multi-reaction monitoring acquisition, and quantified by external standard method. Results The results showed that 50 kinds of antibiotics exhibited good linearity in the range of 0.1-100.0 ng/mL, and the correlation coefficients were all greater than 0.99. The limit of detection ofthe method was 0.1-2.0 µg/kg, the limit of quantitation was 0.5-5.0 μg/kg. Recovery tests were carried out at 3 levels (1 times, 2 times, 10 times of the limit of quantitation) in the blank matrix, the average recoveries of the limit of detection were in the range of 54.83%-120.01%, and all the relative standard deviations (n=6) were 0.08%-9.15%. Conclusion This method has the technical advantages of simple operation process, excellent detection sensitivity, reliable precision, and good reproducibility, it can be applied to rapid screening and qualitative and quantitative detection of multiple antibiotics in dried sea cucumbers.

multifunctional purification column  /  ultra performance liquid chromatography-tandem mass spectrometry  /  dried sea cucumbers  /  antibiotic residues
宫艳艳, 钱亮亮. 超高效液相色谱-串联质谱法结合多功能净化柱测定干海参中50种抗生素残留. 食品安全质量检测学报, 2025 , 16 (14) : 139 -146 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250410001
Yan-Yan GONG, Liang-Liang QIAN. Determination of 50 kinds of antibiotic residues in dried sea cucumbers by multifunctional purification column with ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (14) : 139 -146 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250410001
正文
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0 引言
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海参隶属于棘皮动物门, 是海洋无脊椎动物中的重要类群, 在全球海洋广泛分布。它是高蛋白、低脂肪且不含胆固醇的优质食材, 亦是我国海水养殖行业中占据重要经济地位的代表性品种[1-2]。海参组织中含有丰富的有益活性成分, 具有提升免疫力、预防疾病以及延缓衰老等功效[3]。干海参, 作为海参经不同脱水工艺制成的名贵海产品, 是海参市场的主导产品[4]。近年来, 受市场需求驱动, 海参养殖产业规模与产量持续扩大。在海参养殖、加工及流通全产业链中, 为防控微生物污染, 抗生素使用存在诸多不合理现象, 包括用药指征不明确、用药剂量超标等误用及滥用情况, 给食品安全带来潜在风险[5-7]。根据化学结构特征, 常用抗生素涵盖磺胺类、β-内酰胺类、酰胺醇类、林可酰胺类、喹诺酮类、大环内酯类、四环素类、氨基糖苷类以及硝基呋喃类等典型类别[8], 诸多抗生素已在环境样品以及全球各海洋中被广泛检出[9-10]。食用含有抗生素的食物, 易致使药物在人体内蓄积, 甚至引发耐药性, 过敏反应等, 严重威胁人类健康[11-13]。鉴于抗生素残留对食品安全及公众健康的潜在风险, 建立干海参等食品中抗生素残留的精准检测方法具有重要意义。当前主要检测方法涵盖微生物法[14]、电化学法[15-16]、毛细管电泳法[17-18]、免疫分析技术[19-21]、气相色谱法[22]、气相色谱-串联质谱法[23]、液相色谱法[24-26]、液相色谱-串联质谱法等[27-28]。鉴于抗生素的特性以及对高灵敏度检测的需求, 液相色谱-串联质谱法常被视作抗生素及其代谢产物分析检测的主流手段[29-30], 是一次可检测多种物质的高通量定性定量分析方法也是抗生素以及多种兽药残留分析的发展方向。现有国家标准中对动物源性抗生素的检测多数是针对某一类或某几类抗生素的检测方法, 如四环素类、磺胺类、喹诺酮类、硝基呋喃类、β-内酰胺类都有各自的检测方法, 且氨基糖苷类抗生素易与海参中的酸性黏多糖结合, 常规提取方法难以完全释放目标物, 因此, 本研究开发了一种基于超高效液相色谱-串联质谱法的高通量检测技术, 通过单次进样即可实现干海参中50种抗生素的同步分析。该方法以磺胺类、喹诺酮类、四环素类等典型抗生素为目标物, 构建了集快速筛查、精准定性和准确定量于一体的分析体系, 可有效满足干海参多类别抗生素残留检测需求, 同时也可为水产品质量安全监测提供精准、高效的分析检测方案。
1 材料与方法
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1.1 材料与试剂
干海参购于连云港市海宁路农产品综合市场、连云港市瀛洲路农贸市场、连云港市海鲜蔬菜小商品市场及周边海产品销售店铺。
甲醇、乙腈、甲酸(色谱纯, 德国默克股份两合公司); 氯化钠、无水硫酸钠、乙二胺-N-丙基硅烷(primary- secondary amine, PSA)(分析纯, 国药集团化学试剂有限公司); 抗生素标准物质(磺胺类混标100 μg/mL、喹诺酮类混标100 μg/mL、四环素类混标100 μg/mL、大环内酯类混标100 μg/mL、β-内酰胺类混标100 μg/mL、林可酰胺类混标100 μg/mL、酰胺醇类混标100 μg/mL)(北京曼哈格生物技术有限公司)。
1.2 仪器与设备
SCIEX QTRAP 5500超高效液相色谱-串联质谱仪[配电喷雾离子源(electrospray ionization source, ESI), 上海爱博才思分析仪器贸易有限公司]; Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm)(美国Waters有限公司); LS220A电子分析天平(精度0.001 g, 瑞士普利赛斯有限公司); Vibrax VXR涡旋振荡仪(德国IKA公司); Milli-Q Advantage A10超纯水机(密理博中国有限公司); TGL-16G 高速台式离心机(上海安亭科学仪器厂)。
1.3 实验方法
1.3.1 标准溶液的配制
准确移取磺胺类混标、喹诺酮类混标、四环素类混标、大环内酯类混标、β-内酰胺类混标、酰胺醇类混标各1 mL于100 mL容量瓶, 用甲醇稀释至刻度, 配制成质量浓度为1.0 μg/mL的标准中间液Ⅰ。移取标准中间液Ⅰ 2 mL于10 mL容量瓶, 用50%甲醇稀释至刻度, 配制成浓度为200 ng/mL的标准中间液Ⅱ。分别准确移取标准中间液Ⅱ相应数量, 用经检验不含抗生素的海参空白基质稀释, 混匀, 配制成质量浓度分别为0.1、1.0、2.0、5.0、10.0、20.0、50.0、100.0 ng/mL的系列标准工作液。
1.3.2 样品处理
干海参样品前处理参照GB 31602—2015《食品安全国家标准 干海参》中兽药残留检测要求进行。样品经室温预浸泡24 h、清洗、两次水煮后, 晾至室温, 置于0~10 ℃冰箱中放置20 h后取出, 用滤纸吸去表面水分, 绞碎备用。称取2.0 g样品置于50 mL离心管中, 加入8 mL乙腈水(V:V=50:50)溶液, 涡旋振荡5 min, 超声提取5 min, 8000 r/min离心5 min, 将上清液加载至自填充多功能净化柱上。接收4 mL流出液, 在40 ℃水浴条件下氮吹至约0.5 mL, 用乙腈水溶液定容至1.0 mL, 涡旋混匀后, 经0.22 μm微孔滤膜过滤, 上机测试。
1.3.3 液相色谱条件
Waters ACQUITY UPLC HSS T3色谱柱, 柱温30 ℃; 进样量2 μL; 流速0.3 mL/min; 流动相A为0.1%甲酸水(含5 mmol/L乙酸铵), 流动相B为乙腈。梯度洗脱条件见表1。
1.3.4 质谱条件
离子源选用ESI; 扫描模式设定为正离子模式扫描; 采用多反应监测采集方式(multiple reaction monitoring, MRM); 气帘气压力40 psi; 离子源温度550 ℃; 喷雾气40 psi; 辅助加热气40 psi; 碰撞气9 psi; 电喷雾电压5500 V, 质谱参数见表2。
1.4 数据处理
每组试验至少重复3次, 使用SPSS 20.0软件和Origin Pro 2021软件对数据进行处理分析并绘图。
2 结果与分析
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2.1 质谱和色谱条件的优化
2.1.1 色谱柱的选择
在抗生素分析检测工作中, 反相色谱柱较为常用[31], 本研究对Waters C18 (100 mm×3.0 mm, 1.7 μm)、Waters ACQUITY UPLC HSS T3 (100 mm×2.1 mm, 1.8 μm)和Waters ACQUITY UPLC HSS T3 (50 mm×2.1 mm, 1.7 μm)这3种色谱柱对50种兽药的分离效果进行比较, 结果显示, Waters ACQUITY UPLCHSS T3 (100 mm×2.1 mm, 1.8 μm)色谱柱的分离效果明显, 峰形良好, 无拖尾现象。综合色谱峰形、分离度及柱效等因素, 最终将Waters ACQUITY UPLC HSS T3反相色谱柱(100 mm×2.1 mm, 1.8 μm)确定为实现目标化合物分离的最佳选择。
2.1.2 质谱条件优化
基于流动注射进样方式, 在正离子检测模式下对质量浓度为100.0 ng/mL的50种化合物混标溶液实施母离子(Q1)全扫描分析, 准确识别各目标物的母离子。随后利用二级质谱(MS2)技术, 系统优化调整去簇电压、碰撞电压等关键质谱参数。从各化合物的质谱碎片中选取2组高响应离子对, 分别作为定量与定性分析的特征离子, 详细质谱参数优化结果见表2。液相色谱分离中采用0.1%甲酸水(含5 mmol/L乙酸铵)和乙腈作为流动相, 通过对梯度洗脱优化, 确保目标化合物获得理想的分离度与峰形。
2.2 样品前处理方法的选择
2.2.1 样品制备
食用干制海参时, 通常需要进行发泡处理。实验对比了发泡与不发泡两种情况, 发现干制海参直接进行提取, 需额外补水, 同时, 当加标浓度设定为10.0 μg/kg时, 对比发泡与未发泡海参的回收率, 结果显示发泡海参的回收率普遍更高, 回收率对比情况见图1。
喹诺酮类抗生素(含羧酸和哌嗪基团)、β-内酰胺类抗生素(含β-内酰胺环)及四环素类抗生素(含共轭双键和多个羟基), 均呈现显著的pH依赖性。干海参提取时补水不足可能导致局部 pH偏离最佳范围, 抗生素的稳定性和活性降低。而发泡处理后水分分布均匀, 体系pH稳定性提升, 可推动解离平衡向游离态跃迁, 显著优化萃取效率。此外, 海参基质中富含Ca2+、Mg2+等金属离子, 在未复水状态下, 此类离子易与喹诺酮类抗生素分子中的羧基螯合形成难溶性复合物; 同时, 海参骨骼残留的高钙基质在未充分复水时易与四环素类抗生素发生强烈螯合作用, 生成不溶性复合物。复水操作可稀释金属离子浓度, 减弱螯合作用, 促使药物活性成分更充分释放。低极性、强脂溶性的酰胺醇类抗生素和低极性、易与蛋白质疏水区域结合的大环内酯类抗生素, 在干海参未发泡时, 蛋白质未充分溶胀, 脂质成分和蛋白质疏水空腔紧密包裹药物, 提取溶剂难以渗透, 导致两类抗生素回收率降低; 经发泡处理后, 脂质结构趋向分散状态, 蛋白质浓度随之降低, 基质效应得以减轻, 抗生素更易被有机溶剂萃取。磺胺类和林可酰胺类抗生素属于中等极性药物。其中, 磺胺类抗生素易与基质中蛋白质、金属离子形成氢键或离子键; 林可酰胺类抗生素因分子结构中含有碱性胺基, 可与酸性基质成分形成离子对。干海参未充分复水时, 蛋白质基质保持紧密结构, 致使磺胺类抗生素易通过氢键结合胶原蛋白产生不可逆吸附, 且高极性基质会与磺胺类竞争溶剂, 硫酸软骨素等酸性多糖未充分溶胀时易与林可酰胺类抗生素形成强离子对, 阻碍极性溶剂的提取作用, 导致提取不充分、回收率偏低; 发泡处理后, 基质发生溶胀且结构趋于松散, 吸附作用减弱, 磺胺类抗生素更易从基质中释放, 同时多糖溶解促使离子对解离, 林可酰胺类抗生素回收率亦显著提高。
2.2.2 提取溶剂的选择
开展干制海参内多种不同类型抗生素的同步测定研究工作, 在选用提取溶剂时, 需综合考量待测物质在溶剂中的溶解度、溶剂与基质的浸透效果等因素。同时由于抗生素稳定性较差, 提取溶剂选择尤为关键。在检测抗生素类化合物时, 乙腈、正己烷、甲醇、乙酸乙酯、二氯甲烷等是常用的提取溶剂。经乙酸乙酯、二氯甲烷、甲醇提取后, 样品溶液中油脂含量较高, 且杂质去除效果不理想。乙腈属于极性溶剂, 将其用作提取溶剂时, 能够有效避免样品中的脂肪被过度提取, 同时对蛋白质沉淀也能起到良好效果。添加一定比例的水相, 可防止有机相比例过高致使提取的杂质过多, 进而堵塞柱子, 在调整乙腈极性的同时, 兼顾多种不同极性的目标化合物, 该方法可显著提升目标化合物的富集效率, 为后续的定性定量分析提供可靠保障[32]。综合回收率与基质效应等多方面因素, 本研究将体积分数50%乙腈水溶液选定为目标化合物的最佳提取剂。
2.2.3 净化方式
本研究旨在建立一套快速进行抗生素筛查的实验方案, 考虑到传统的净化方式难以兼容不同种类抗生素的处理, 因此, 开展新型前处理净化方法的研究与优化开发。针对基质中干扰因素, 主要为脂溶性物质和蛋白质类物质, 分别筛选用于净化蛋白和脂肪的相关材料, 进行复合净化小柱的填充工作。通过对空白样品在10.0 μg/kg水平下进行加标回收实验, 以加标回收效果作为评估依据, 对比阳离子氧化锆、C18、PSA、中性氧化铝等多种净化材料复合填柱的效果, 确定合适的填充材料及比例。选取干海参基质空白为载体, 开展50种化合物的加标回收率实验, 以此选定合适的多功能净化柱。结果表明: 样品经多功能净化柱净化后, 多数目标物质的基质回收率处于80%~110%区间, 满足实验净化的需求。
2.2.4 基质效应评估
本研究进行了基质效应的评估时发现, 干制海参由于蛋白质基质干扰极为严重, 试剂标准曲线难以满足实验需求, 因此采用空白基质配制标准溶液, 获得校正曲线的方式, 以降低干制海参的基质效应。
2.3 方法学验证
2.3.1 标准曲线、检出限和定量限
在实验设定的质谱分析条件下, 以空白样品基质配制的50种抗生素标准溶液, 当质量浓度处于0.1~100.0 ng/mL 范围时, 浓度与其对应的峰面积线性关系良好, 所有组分相关系数均大于0.99, 具体数据见表3。
2.3.2 检出限和定量限
在基质空白样品中进行加标, 采用定量离子3倍信噪比(S/N=3)和10倍信噪比(S/N=10)分别进行计算, 50 种抗生素的检出限和定量限分别为0.1~2.0 μg/kg、0.5~5.0 μg/kg, 详细数据见表3。
2.3.3 基质加标回收率
对50种化合物进行基质加标, 加标1为1倍定量限(n=6), 加标2为2倍定量限(n=3), 加标3为10倍定量限(n=3)。检测结果表明, 加标回收率符合预期标准, 仅有少数化合物的回收率小于60%或大于120%, 例如氨苄西林。考虑到本研究方法分析的抗生素种类繁多, 各化合物结构和极性差异较大[33], 存在少数回收率欠佳的抗生素属于正常现象。对于回收率不理想的待测组分, 该方法的检出限低于我国限量标准, 所以即使回收率较差, 也能确保检出率, 相关数据见表3。
2.3.4 基质加标精密度
以基质1倍定量限进行6平行加标, 利用峰面积计算精密度, 所得精密度均小于10%, 满足检验要求, 数据见表3。
2.3.5 实际样本检测结果
从干制海产品市场和店铺购买46份海参样本, 利用所建立的方法进行样本检测, 检出阳性样本3份, 其中2份样本检出喹诺酮类抗生素, 1份样本检出磺胺类抗生素, 见图2, 将检测结果与《农业部1077号公告-1-2008》中所用方法对比, 结果基本一致。
3 结论
收起
本研究成功建立了同时测定海参基质组织中50种抗生素的超高效液相色谱-串联质谱分析测定方法。实验选用自填多功能净化柱, 通过对基质50种抗生素进行加标回收实验, 优化填充材料和配比, 最终确定自填充多层净化柱为最佳净化方式。方法仅需一次前处理, 便可实现对喹诺酮类、大环内酯类、磺胺类、β-内酰胺类、酰胺醇类、林可酰胺类、四环素类等多类抗生素的检测。此方法不仅操作便捷、检验效率高、结论精准可靠, 还能大幅节约有机试剂, 人力与时间成本双降, 检测效率实现跨越式提升。该方法符合兽药残留检测分析从传统方法向高通量、便捷前处理发展的趋势, 具备较高的实际应用价值。
基金
收起
  • 江苏省市场监督管理局技术能力提升项目(NL2021047)
  • 连云港市科技计划项目(SF2331)
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2025年第16卷第14期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250410001
  • 接收时间：2025-04-10
  • 首发时间：2026-01-07
  • 出版时间：2025-07-25
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  • 收稿日期：2025-04-10
基金
江苏省市场监督管理局技术能力提升项目(NL2021047)
连云港市科技计划项目(SF2331)
作者信息
    1 连云港市食品药品检验检测中心, 连云港 222000
    2 连云港市质量技术综合检验检测中心, 连云港 222000

通讯作者:

*钱亮亮(1984—), 男, 正高级工程师, 主要研究方向为食品检测与质量安全控制。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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