Article(id=1217529314380271777, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250219005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1739894400000, receivedDateStr=2025-02-19, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768211209148, onlineDateStr=2026-01-12, pubDate=1752508800000, pubDateStr=2025-07-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768211209148, onlineIssueDateStr=2026-01-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768211209148, creator=13701087609, updateTime=1768211209148, updator=13701087609, issue=Issue{id=1217529305693864468, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='13', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768211207077, creator=13701087609, updateTime=1768212057891, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217532874337730593, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217532874337730594, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=87, endPage=92, ext={EN=ArticleExt(id=1217529315219132687, articleId=1217529314380271777, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Rapid detection of enrofloxacin residues in complex mixed matrix of Hainan’s special “soil-vegetable” system by ultra performance liquid chromatography-tandem mass spectrometry, columnId=1217529311867883548, journalTitle=Journal of Food Safety & Quality, columnName=Highlight: Analysis and Monitoring of Toxic and Harmful Substances in Food, runingTitle=null, highlight=null, articleAbstract=
Objective To establish an analytical method for the determination of enrofloxacin residues in complex mixed matrix of the “soil-vegetable” system by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was subjected to vortex ultrasonic extraction with acidified acetonitrile extract [containing 5% ethylene diamine tetraacetic acid (EDTA)-Mcllvaine buffer solution], settling with centrifugation, getting solvent conversion and being filtered by 0.22 μm nylon filter membrane. The mobile phase was composed of acetonitrile and 0.1% formic acid aqueous solution (containing 2 mmol/L ammonium acetate), and the mixture was subjected to Waters ACQUITY UPLC ® BEH C18 chromatographic column (2.1 mm×100 mm, 1.7 μm) gradient elution separation, using mass spectrometry as a detector for qualitative and quantitative analysis of enrofloxacin. Results In the mass concentration range of 1-200 ng/mL, the standard curve showed a good linear relationship (correlation coefficient=0.9996), the limit of detection of the method was 0.11 μg/kg, the recovery rates ranged from 87.4% to 103.3%, and the relative standard deviations (RSDs) were 0.4% to 4.0% (n=6). Conclusion This method has fast analysis speed, high accuracy and good repeatability, and is suitable for the detection of enrofloxacin residues in complex mixed matrix of the “soil-vegetable” system. It also has the potential to indirectly reveal the risk of antibiotic resistance genes (ARGs) contamination in the system.
, correspAuthors=Bin WANG, 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=Chao-Feng LIU, Xiao-Yu GUO, Hong-Miao CHEN, Rui KANG, Yu-Ling ZHOU, Bin WANG), CN=ArticleExt(id=1217529316007661935, articleId=1217529314380271777, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=超高效液相色谱-串联质谱法快速检测海南特色“土壤-蔬菜”系统复杂混合基质中恩诺沙星残留, columnId=1217529312056627244, journalTitle=食品安全质量检测学报, columnName=本期重点:食品中有毒有害物质分析与监测, runingTitle=null, highlight=null, articleAbstract=
目的 建立基于超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定海南特色“土壤-蔬菜”系统中复杂混合基质恩诺沙星残留的分析方法。
方法 样品经酸化乙腈提取液[含5%乙二胺四乙酸(ethylene diamine tetraacetic acid, EDTA)-Mcllvaine缓冲溶液]涡旋超声提取, 离心沉降, 溶剂转换, 0.22 μm尼龙滤膜过滤后, 以乙腈和0.1%甲酸水溶液(含2 mmol/L乙酸铵)为流动相, 经Waters ACQUITY UPLC® BEH C
18色谱柱(2.1 mm×100 mm, 1.7 μm)梯度洗脱分离, 使用质谱仪作为检测器对恩诺沙星进行定性定量。
结果 在1~200 ng/mL的质量浓度范围中, 标准曲线线性关系良好(相关系数为0.9996), 方法的检出限为0.11 μg/kg, 加标回收率范围为87.4%~103.3%, 相对标准偏差(relative standard deviations, RSDs)为0.4%~4.0% (
n=6)。
结论 该分析方法快速、准确、重复性良好, 适用于“土壤-蔬菜”系统复杂混合基质中恩诺沙星残留的检测, 拥有间接揭示系统中抗生素耐药性基因(antibiotic resistance genes, ARGs)污染风险的潜力。, correspAuthors=王彬, authorNote=null, correspAuthorsNote=
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, authorsList=刘超烽, 郭晓宇, 陈虹妙, 康蕊, 周玉玲, 王彬)}, authors=[Author(id=1217901249542931397, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=1071147506@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1217901249651983320, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901249542931397, language=EN, stringName=Chao-Feng LIU, firstName=Chao-Feng, middleName=null, lastName=LIU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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1 Institute of Food Testing, Hainan Academy of Inspection and Testing, Haikou 570311, China
2 Key Laboratory of Tropical Fruits and Vegetables Quality and Safety, State Administration for Market Regulation, Haikou 570311, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1217901249840727013, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901249542931397, language=CN, stringName=刘超烽, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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1 海南省检验检测研究院食品检验检测中心, 海口 570311
2 国家市场监督管理总局重点实验室(热带果蔬质量与安全), 海口 570311, bio={"content":"
刘超烽(1996—), 男, 硕士, 工程师, 主要研究方向为食品安全及色谱分析。E-mail: 1071147506@qq.com
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刘超烽(1996—), 男, 硕士, 工程师, 主要研究方向为食品安全及色谱分析。E-mail: 1071147506@qq.com
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1 Institute of Food Testing, Hainan Academy of Inspection and Testing, Haikou 570311, China
2 Key Laboratory of Tropical Fruits and Vegetables Quality and Safety, State Administration for Market Regulation, Haikou 570311, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1217901250369208323, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901249966556141, language=CN, stringName=郭晓宇, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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1 海南省检验检测研究院食品检验检测中心, 海口 570311
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1 海南省检验检测研究院食品检验检测中心, 海口 570311)]), AuthorCompany(id=1217901247827461024, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=2, ext=[AuthorCompanyExt(id=1217901247840043936, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247827461024, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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1 Institute of Food Testing, Hainan Academy of Inspection and Testing, Haikou 570311, China
2 Key Laboratory of Tropical Fruits and Vegetables Quality and Safety, State Administration for Market Regulation, Haikou 570311, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1217901250704752676, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901250474065935, language=CN, stringName=陈虹妙, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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1 海南省检验检测研究院食品检验检测中心, 海口 570311
2 国家市场监督管理总局重点实验室(热带果蔬质量与安全), 海口 570311, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1217901247668077459, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=1, ext=[AuthorCompanyExt(id=1217901247684854677, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247668077459, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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1 海南省检验检测研究院食品检验检测中心, 海口 570311)]), AuthorCompany(id=1217901247827461024, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=2, ext=[AuthorCompanyExt(id=1217901247840043936, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247827461024, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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1 Institute of Food Testing, Hainan Academy of Inspection and Testing, Haikou 570311, China
2 Key Laboratory of Tropical Fruits and Vegetables Quality and Safety, State Administration for Market Regulation, Haikou 570311, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1217901251082240078, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901250805415985, language=CN, stringName=康蕊, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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1 海南省检验检测研究院食品检验检测中心, 海口 570311
2 国家市场监督管理总局重点实验室(热带果蔬质量与安全), 海口 570311, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1217901247668077459, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=1, ext=[AuthorCompanyExt(id=1217901247684854677, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247668077459, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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2, 3, address=
2 Key Laboratory of Tropical Fruits and Vegetables Quality and Safety, State Administration for Market Regulation, Haikou 570311, China
3 Institute of Quality and Standardization, Hainan Academy of Inspection and Testing, Haikou 570311, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1217901251463921790, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, authorId=1217901251195486300, language=CN, stringName=周玉玲, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=
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33(10): 1009-1020., articleTitle=Matrix effects in liquid chromatography-mass spectrometry analysis techniques, refAbstract=null)], funds=[Fund(id=1217901256409006596, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, awardId=ZZ-2024007, language=CN, fundingSource=国家市场监督管理总局重点实验室(热带果蔬质量与安全)自主研究课题项目(ZZ-2024007), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1217901247668077459, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=1, ext=[AuthorCompanyExt(id=1217901247684854677, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247668077459, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
1 Institute of Food Testing, Hainan Academy of Inspection and Testing, Haikou 570311, China), AuthorCompanyExt(id=1217901247705826198, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247668077459, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
1 海南省检验检测研究院食品检验检测中心, 海口 570311)]), AuthorCompany(id=1217901247827461024, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=2, ext=[AuthorCompanyExt(id=1217901247840043936, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901247827461024, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
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3 Institute of Quality and Standardization, Hainan Academy of Inspection and Testing, Haikou 570311, China), AuthorCompanyExt(id=1217901248091702186, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901248049759141, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
3 海南省检验检测研究院质量技术监督标准与信息所, 海口 570311)]), AuthorCompany(id=1217901249412907961, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, xref=4, ext=[AuthorCompanyExt(id=1217901249421296570, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901249412907961, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
4 Center for Food Evaluation, Hainan Academy of Inspection and Testing, Haikou 570311, China), AuthorCompanyExt(id=1217901249429685178, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, companyId=1217901249412907961, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=
4 海南省检验检测研究院食品审评中心, 海口 570311)])], figs=[ArticleFig(id=1217901254894862696, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=EN, label=Fig.1, caption=
Structural formula of enrofloxacin, figureFileSmall=W3+wvAG3Hpse0aGKPg5LAA==, figureFileBig=9FdpGittzGnDVfrF4aMNlw==, tableContent=null), ArticleFig(id=1217901255071023480, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=CN, label=图1, caption=
恩诺沙星结构式, figureFileSmall=W3+wvAG3Hpse0aGKPg5LAA==, figureFileBig=9FdpGittzGnDVfrF4aMNlw==, tableContent=null), ArticleFig(id=1217901255247184266, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=EN, label=Fig.2, caption=
Effects of EDTA-Mcllvaine buffer solution content on the extraction results of enrofloxacin in mixed matrices (n=6), figureFileSmall=gjNnGoOmJ5VVDrP8iB/wwA==, figureFileBig=R6KY1V7GlWUiaEdVBKa2hw==, tableContent=null), ArticleFig(id=1217901255364624785, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=CN, label=图2, caption=
EDTA-Mcllvaine缓冲溶液含量对复合基质中恩诺沙星提取效果的影响(n=6), figureFileSmall=gjNnGoOmJ5VVDrP8iB/wwA==, figureFileBig=R6KY1V7GlWUiaEdVBKa2hw==, tableContent=null), ArticleFig(id=1217901255532396963, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=EN, label=Table 1, caption=
Program of gradient elution
, figureFileSmall=null, figureFileBig=null, tableContent=
| 时间/min | 流动相A/% | 流动相B/% |
| 起始 | 90 | 10 |
| 0.3 | 90 | 10 |
| 1.0 | 60 | 40 |
| 2.8 | 10 | 90 |
| 3.3 | 10 | 90 |
| 3.4 | 90 | 10 |
| 4.0 | 90 | 10 |
), ArticleFig(id=1217901255654031795, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=CN, label=表1, caption=
梯度洗脱程序
, figureFileSmall=null, figureFileBig=null, tableContent=
| 时间/min | 流动相A/% | 流动相B/% |
| 起始 | 90 | 10 |
| 0.3 | 90 | 10 |
| 1.0 | 60 | 40 |
| 2.8 | 10 | 90 |
| 3.3 | 10 | 90 |
| 3.4 | 90 | 10 |
| 4.0 | 90 | 10 |
), ArticleFig(id=1217901255779860935, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=EN, label=Table 2, caption=
Parent ion, daughter ion, cone voltage and collision energy of enrofloxacin
, figureFileSmall=null, figureFileBig=null, tableContent=
| 化合物 | 母离子(m/z) | 子离子(m/z) | 锥孔电压/V | 碰撞能量/eV |
| 恩诺沙星 | 360 | 360>245 | 30 | 24 |
| 360>316* | 30 | 19 |
| 恩诺沙星-D5 | 365 | 365>321 | 35 | 19 |
), ArticleFig(id=1217901255880524244, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=CN, label=表2, caption=
恩诺沙星母离子、子离子、锥孔电压和碰撞能量
, figureFileSmall=null, figureFileBig=null, tableContent=
| 化合物 | 母离子(m/z) | 子离子(m/z) | 锥孔电压/V | 碰撞能量/eV |
| 恩诺沙星 | 360 | 360>245 | 30 | 24 |
| 360>316* | 30 | 19 |
| 恩诺沙星-D5 | 365 | 365>321 | 35 | 19 |
), ArticleFig(id=1217901256014741986, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=EN, label=Table 3, caption=
Results of recoveries of enrofloxacin in the “soil-vegetable” system (n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 基质种类 | 添加浓度 /(μg/kg) | 回收率 /% | RSDs /% |
| 地瓜叶 | 10 | 92.3 | 1.3 |
| 100 | 101.9 | 1.5 |
| 500 | 88.0 | 1.9 |
| 桥头地瓜 | 10 | 95.3 | 3.2 |
| 100 | 100.9 | 0.4 |
| 500 | 87.4 | 2.2 |
| 土壤 | 10 | 100.2 | 4.0 |
| 100 | 103.3 | 1.7 |
| 500 | 91.6 | 4.0 |
| 复合基质 | 10 | 94.2 | 1.2 |
| 100 | 100.4 | 3.6 |
| 500 | 94.3 | 1.8 |
), ArticleFig(id=1217901256157348333, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529314380271777, language=CN, label=表3, caption=
“土壤-蔬菜”系统中恩诺沙星的加标回收结果(n=6)
, figureFileSmall=null, figureFileBig=null, tableContent=
| 基质种类 | 添加浓度 /(μg/kg) | 回收率 /% | RSDs /% |
| 地瓜叶 | 10 | 92.3 | 1.3 |
| 100 | 101.9 | 1.5 |
| 500 | 88.0 | 1.9 |
| 桥头地瓜 | 10 | 95.3 | 3.2 |
| 100 | 100.9 | 0.4 |
| 500 | 87.4 | 2.2 |
| 土壤 | 10 | 100.2 | 4.0 |
| 100 | 103.3 | 1.7 |
| 500 | 91.6 | 4.0 |
| 复合基质 | 10 | 94.2 | 1.2 |
| 100 | 100.4 | 3.6 |
| 500 | 94.3 | 1.8 |
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