Article(id=1321413621167538745, tenantId=1146029695717560320, journalId=1296801528146919473, issueId=1321413606437139054, articleNumber=null, orderNo=null, doi=10.12377/1671-4393.25.01.12, pmid=null, cstr=null, oa=null, hot=0, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=null, receivedDateStr=null, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1792979157964, onlineDateStr=2026-10-26, pubDate=null, pubDateStr=null, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792979157964, onlineIssueDateStr=2026-10-26, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792979157964, creator=13701087609, updateTime=1792979157964, updator=13701087609, issue=Issue{id=1321413606437139054, tenantId=1146029695717560320, journalId=1296801528146919473, year='2025', volume='', issue='1', pageStart='0', pageEnd='120', issueExtLink='null', onlineDate='null', pubDate='1737734400000', pubDateStr='2025-01-25', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792979154452, creator='13701087609', updateTime=1792979201578, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1321413804169220826, tenantId=1146029695717560320, journalId=1296801528146919473, issueId=1321413606437139054, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1321413804169220827, tenantId=1146029695717560320, journalId=1296801528146919473, issueId=1321413606437139054, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=71, endPage=79, ext={EN=ArticleExt(id=1321413621515665979, articleId=1321413621167538745, tenantId=1146029695717560320, journalId=1296801528146919473, language=EN, title=Determination of 83 Pesticide Residues in Raw Milk by High Performance Liquid Chromatography Tandem Mass Spectrometry, columnId=1297134031947194991, journalTitle=China Dairy, columnName=QUALITY CONTROL, runingTitle=null, highlight=null, articleAbstract=[Objective] To establish a high-performance liquid chromatography tandem mass spectrometry analysis method for multiple pesticide residues in raw milk.[Method] Raw milk samples were extracted with acetonitrile,purified with 150 mg of N-propylethylenediamine(PSA),900 mg of magnesium sulfate and 15 mg of C18,and then eluted with liquid phase gradient.The samples were detected by electric spray(ESI+/ESI-),and quantified by matrix matching external standard method.A rapid qualitative and quantitative analysis method for 83 pesticide residues in raw milk was established.[Result] The results of method validation showed that 83 pesticide residues exhibited good linearity within the range of 0.5 μg/L to 100 μg/L,with a correlation coefficient R2 >0.99.The recovery rate of adding at three levels(0.010 mg/L,0.020 mg/L,0.100 mg/L) is 32%~134%,with a relative standard deviation of 0.3%~8.5%.[Conclusion] This experimental method is simple to operate,time-consuming,and suitable for rapid screening and quantitative analysis of pesticide residues in raw milk.It has practical application value. Using this method,83 pesticide residues were detected in 50 batches of raw milk,all of which meet the requirements of the GB 2763—2021 National Food Safety Standard Maximum Residue Limits for Pesticides in Food for raw milk., authors=FAN Guangcai1 , ZHOU Huan1 , SONG Yanmei1 , LI Qingqing2 , LUO Ming1 , MA Jing1 , XIA Zhongyue1,* , authorsList=FAN Guangcai, ZHOU Huan, SONG Yanmei, LI Qingqing, LUO Ming, MA Jing, XIA Zhongyue, authorCompany=1 New Hope Dairy Co.,Ltd.,Chengdu Sichuan 610000; 2 Chengdu Jinfu Monkey Food Co.,Ltd.,Chengdu Sichuan 610000, correspAuthors=null, 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, fund=null), CN=ArticleExt(id=1321413621406614074, articleId=1321413621167538745, tenantId=1146029695717560320, journalId=1296801528146919473, language=CN, title=高效液相色谱串联质谱法测定生乳中83 种农药残留, columnId=1297134032135938673, journalTitle=中国乳业, columnName=质量安全, runingTitle=null, highlight=null, articleAbstract=[目的] 建立一种生乳中多种农药残留快速定性定量的高效液相色谱串联质谱分析方法。[方法] 生乳样品经乙腈提取后,用含有150 mg N-丙基乙二胺(PSA)、900 mg硫酸镁、15 mg C18净化,后经液相梯度洗脱。在电喷雾(ESI+/ESI-)下使用质谱进行检测,通过基质匹配外标法定量,建立生乳中83 种农药残留快速定性定量分析方法。[结果] 经验证,83 种农药残留在0.5~100 μg/L范围内线性良好,相关系数R2 >0.99。在 3 水平添加(0.010 mg/L、0.020 mg/L、0.100 mg/L)回收率为32%~134%,相对标准偏差为0.3%~8.5%。[结论] 该试验方法操作简单、耗时短,适用于生乳中农药残留快速筛查和定量分析,具有实际应用价值。用该方法检测50 批次生乳中83 种农药残留,均满足《GB 2763—2021 食品安全国家标准 食品中农药最大残留限量》对生乳的要求。, authors=范光彩1 , 周欢1 , 宋艳梅1 , 李清清2 , 骆敏1 , 马静1 , 夏忠悦1,* , authorsList=范光彩, 周欢, 宋艳梅, 李清清, 骆敏, 马静, 夏忠悦, authorCompany=1 新希望乳业股份有限公司,四川成都 610000; 2 成都市金福猴食品股份有限公司,四川成都 610000, correspAuthors=* 夏忠悦(1971-),女,四川内江人,本科,高级工程师,研究方向为乳制品质量安全及控制。, authorNote=范光彩(1995-),男,四川广元人,本科,中级工程师,研究方向为乳制品质量安全及控制;周 欢(1996-),女,四川南充人,本科,中级工程师,研究方向为乳制品质量安全及控制;宋艳梅(1982-),女,四川乐山人,本科,高级工程师,研究方向为乳制品质量安全及控制;李清清(1993-),女,四川绵阳人,本科,中级工程师,研究方向为调味品质量安全及控制;骆 敏(1992-),女,四川内江人,本科,中级工程师,研究方向为乳制品质量安全及控制;马 静(1994-),女,河北唐山人,硕士,中级工程师,研究方向为乳制品质量安全及控制。, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=5QKDuPv0rj85z2qyfuS43A==, pdfFileSize=1270243, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=四川省科技计划资助,改善慢性肠道炎症益生菌的作用机制及其产业化研究,2024YFHZ0007)}, authors=null, keywords=[Keyword(id=1321413621649883708, tenantId=1146029695717560320, journalId=1296801528146919473, articleId=1321413621167538745, language=CN, orderNo=1, keyword=高效液相色谱串联质谱), Keyword(id=1321413621721186877, 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interPubPlatformUrl=null), detailUrlCn=https://castjournals.cast.org.cn/joweb/zgry/CN/10.12377/1671-4393.25.01.12, detailUrlEn=https://castjournals.cast.org.cn/joweb/zgry/EN/10.12377/1671-4393.25.01.12, pdfUrlCn=https://castjournals.cast.org.cn/joweb/zgry/CN/PDF/10.12377/1671-4393.25.01.12, pdfUrlEn=https://castjournals.cast.org.cn/joweb/zgry/EN/PDF/10.12377/1671-4393.25.01.12, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, previewStatus=0, delFlag=0, hasFullText=0, orderTime=1792979157964, fullTextJson=null, articleText=null, reference=[1] 李菊颖,何健,吴文铸,等.超高效液相色谱-串联质谱法测定氟啶虫胺腈在黄瓜花粉上的残留[J].农药,2016,55(7):524-526. [2] 田海,冯玉洁,张艳玲,等.超高效液相色谱串联质谱法测定鸡肉中噻节因残留[J].现代农药,2017,16(4):39-41. [3] 张云,程立军,侯杰,等.UPLC-MS/MS测定葡萄酒中3 种双酰胺类杀虫剂[J].中国酿造,2016,35(9):172-175. [4] 陈倩娟. 超高效液相色谱-串联质谱法测定黄豆中丙硫菌唑和甲氧咪草烟[J].食品工程,2017(4):44-46,49. [5] 毛佳,代雪芳,李文希,等.超高效液相色谱-串联质谱法测定动物源食品中敌草腈及其代谢物残留[J].农药,2019,58(9):664-667. [6] 张月,韩丙军,李萍萍,等.超高效液相色谱-串联质谱法测定氟噻唑吡乙酮及其代谢产物在热带水果中的残留量[J].分析科学学报,2020,36(3):431-434. [7] 钟青,罗逢健,陈宗懋,等.超高效液相色谱-三重四极杆串联质谱法分析茶叶中联苯肼酯残留与风险评估[J].质谱学报,2019,40(1):32-41. [8] 马有宁,陈铭学,曹赵云,等.高效液相色谱-串联质谱法分析蔬菜中残留的麦草畏[J].农药学学报,2012,14(3):349-352. [9] 张缙,杨黎忠,林立毅,等.高效液相色谱-串联质谱法测定食品中多杀菌素A和D的残留量[J].色谱,2011,29(7):637-642. [10] 韩超,杨兰花,陈祥准,等.葡萄酒中多种吡唑类杀菌剂的固相萃取-液相色谱-串联质谱检测方法[P].浙江省:CN104713977B,2016-05-11. [11] 胡礼,王胜翔,薄瑞.氯丙嘧啶酸原药及其杂质的高效液相色谱-质谱联用法分析[J].农药科学与管理,2011,32(2):45-47. [12] GB 23200.121—2021 食品安全国家标准植物源性食品中331 种农药及其代谢物残留量的测定液相色谱—质谱联用法[S]. [13] GB/T 20769—2008 水果和蔬菜中450 种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. [14] GB/T 20770—2008 粮谷中486 种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. [15] GB/T 23204—2008 茶叶中519 种农药及相关化学品残留量的测定气相色谱-质谱法[S]. [16] GB 23200.8—2016 食品安全国家标准水果和蔬菜中500 种农药及相关化学品残留量的测定气相色谱-质谱法[S]. [17] NY/T1434—2007 蔬菜中2,4-D等13 种除草剂多残留的测定液相色谱质谱法[S]. [18] 蔡振辉. QuEChERS结合GC-MS/MS检测食用菌中20 种有机磷农药的基质效应[J].亚热带农业研究,2022,18(2):136-141. [19] 党娟. 基质效应对六盘水6 种蔬菜中20 种农药残留检测的影响[J].农技服务,2022,39(6):67-72. [20] 王连珠,王瑞龙,王登飞,等.QuEChERS-LC-MS/MS测定果蔬中氟吡呋喃酮方法优化及基质效应的消除[J].现代食品科技,2020,36(8):347-353.)
中国乳业
|质量安全
2025
,
(1) :
71
-79
高效液相色谱串联质谱法测定生乳中83 种农药残留
全屏
范光彩1 , 周欢1 , 宋艳梅1 , 李清清2 , 骆敏1 , 马静1 , 夏忠悦1,*
作者信息
1 新希望乳业股份有限公司,四川成都 610000; 2 成都市金福猴食品股份有限公司,四川成都 610000
通讯作者:
* 夏忠悦(1971-),女,四川内江人,本科,高级工程师,研究方向为乳制品质量安全及控制。
作者简介:
范光彩(1995-),男,四川广元人,本科,中级工程师,研究方向为乳制品质量安全及控制;周 欢(1996-),女,四川南充人,本科,中级工程师,研究方向为乳制品质量安全及控制;宋艳梅(1982-),女,四川乐山人,本科,高级工程师,研究方向为乳制品质量安全及控制;李清清(1993-),女,四川绵阳人,本科,中级工程师,研究方向为调味品质量安全及控制;骆 敏(1992-),女,四川内江人,本科,中级工程师,研究方向为乳制品质量安全及控制;马 静(1994-),女,河北唐山人,硕士,中级工程师,研究方向为乳制品质量安全及控制。
Determination of 83 Pesticide Residues in Raw Milk by High Performance Liquid Chromatography Tandem Mass Spectrometry
FAN Guangcai1 , ZHOU Huan1 , SONG Yanmei1 , LI Qingqing2 , LUO Ming1 , MA Jing1 , XIA Zhongyue1,*
Affiliations
1 New Hope Dairy Co.,Ltd.,Chengdu Sichuan 610000; 2 Chengdu Jinfu Monkey Food Co.,Ltd.,Chengdu Sichuan 610000
doi: 10.12377/1671-4393.25.01.12
文章导航
[目的] 建立一种生乳中多种农药残留快速定性定量的高效液相色谱串联质谱分析方法。[方法] 生乳样品经乙腈提取后,用含有150 mg N-丙基乙二胺(PSA)、900 mg硫酸镁、15 mg C18净化,后经液相梯度洗脱。在电喷雾(ESI+/ESI-)下使用质谱进行检测,通过基质匹配外标法定量,建立生乳中83 种农药残留快速定性定量分析方法。[结果] 经验证,83 种农药残留在0.5~100 μg/L范围内线性良好,相关系数R2 >0.99。在 3 水平添加(0.010 mg/L、0.020 mg/L、0.100 mg/L)回收率为32%~134%,相对标准偏差为0.3%~8.5%。[结论] 该试验方法操作简单、耗时短,适用于生乳中农药残留快速筛查和定量分析,具有实际应用价值。用该方法检测50 批次生乳中83 种农药残留,均满足《GB 2763—2021 食品安全国家标准 食品中农药最大残留限量》对生乳的要求。
[Objective] To establish a high-performance liquid chromatography tandem mass spectrometry analysis method for multiple pesticide residues in raw milk.[Method] Raw milk samples were extracted with acetonitrile,purified with 150 mg of N-propylethylenediamine(PSA),900 mg of magnesium sulfate and 15 mg of C18,and then eluted with liquid phase gradient.The samples were detected by electric spray(ESI+/ESI-),and quantified by matrix matching external standard method.A rapid qualitative and quantitative analysis method for 83 pesticide residues in raw milk was established.[Result] The results of method validation showed that 83 pesticide residues exhibited good linearity within the range of 0.5 μg/L to 100 μg/L,with a correlation coefficient R2 >0.99.The recovery rate of adding at three levels(0.010 mg/L,0.020 mg/L,0.100 mg/L) is 32%~134%,with a relative standard deviation of 0.3%~8.5%.[Conclusion] This experimental method is simple to operate,time-consuming,and suitable for rapid screening and quantitative analysis of pesticide residues in raw milk.It has practical application value. Using this method,83 pesticide residues were detected in 50 batches of raw milk,all of which meet the requirements of the GB 2763—2021 National Food Safety Standard Maximum Residue Limits for Pesticides in Food for raw milk.
HPLC-MS/MS
/
pesticide residue
/
raw milk
范光彩, 周欢, 宋艳梅, 李清清, 骆敏, 马静, 夏忠悦.
高效液相色谱串联质谱法测定生乳中83 种农药残留.
中国乳业,
2025
,
(1)
: 71
-79
.
DOI: 10.12377/1671-4393.25.01.12
FAN Guangcai, ZHOU Huan, SONG Yanmei, LI Qingqing, LUO Ming, MA Jing, XIA Zhongyue.
Determination of 83 Pesticide Residues in Raw Milk by High Performance Liquid Chromatography Tandem Mass Spectrometry[J].
China Dairy ,
2025
,
(1)
: 71
-79
.
DOI: 10.12377/1671-4393.25.01.12
四川省科技计划资助,改善慢性肠道炎症益生菌的作用机制及其产业化研究,2024YFHZ0007
参考文献
引证文献
[1] 李菊颖,何健,吴文铸,等.超高效液相色谱-串联质谱法测定氟啶虫胺腈在黄瓜花粉上的残留[J].农药,2016,55(7):524-526. [2] 田海,冯玉洁,张艳玲,等.超高效液相色谱串联质谱法测定鸡肉中噻节因残留[J].现代农药,2017,16(4):39-41. [3] 张云,程立军,侯杰,等.UPLC-MS/MS测定葡萄酒中3 种双酰胺类杀虫剂[J].中国酿造,2016,35(9):172-175. [4] 陈倩娟. 超高效液相色谱-串联质谱法测定黄豆中丙硫菌唑和甲氧咪草烟[J].食品工程,2017(4):44-46,49. [5] 毛佳,代雪芳,李文希,等.超高效液相色谱-串联质谱法测定动物源食品中敌草腈及其代谢物残留[J].农药,2019,58(9):664-667. [6] 张月,韩丙军,李萍萍,等.超高效液相色谱-串联质谱法测定氟噻唑吡乙酮及其代谢产物在热带水果中的残留量[J].分析科学学报,2020,36(3):431-434. [7] 钟青,罗逢健,陈宗懋,等.超高效液相色谱-三重四极杆串联质谱法分析茶叶中联苯肼酯残留与风险评估[J].质谱学报,2019,40(1):32-41. [8] 马有宁,陈铭学,曹赵云,等.高效液相色谱-串联质谱法分析蔬菜中残留的麦草畏[J].农药学学报,2012,14(3):349-352. [9] 张缙,杨黎忠,林立毅,等.高效液相色谱-串联质谱法测定食品中多杀菌素A和D的残留量[J].色谱,2011,29(7):637-642. [10] 韩超,杨兰花,陈祥准,等.葡萄酒中多种吡唑类杀菌剂的固相萃取-液相色谱-串联质谱检测方法[P].浙江省:CN104713977B,2016-05-11. [11] 胡礼,王胜翔,薄瑞.氯丙嘧啶酸原药及其杂质的高效液相色谱-质谱联用法分析[J].农药科学与管理,2011,32(2):45-47. [12] GB 23200.121—2021 食品安全国家标准植物源性食品中331 种农药及其代谢物残留量的测定液相色谱—质谱联用法[S]. [13] GB/T 20769—2008 水果和蔬菜中450 种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. [14] GB/T 20770—2008 粮谷中486 种农药及相关化学品残留量的测定液相色谱-串联质谱法[S]. [15] GB/T 23204—2008 茶叶中519 种农药及相关化学品残留量的测定气相色谱-质谱法[S]. [16] GB 23200.8—2016 食品安全国家标准水果和蔬菜中500 种农药及相关化学品残留量的测定气相色谱-质谱法[S]. [17] NY/T1434—2007 蔬菜中2,4-D等13 种除草剂多残留的测定液相色谱质谱法[S]. [18] 蔡振辉. QuEChERS结合GC-MS/MS检测食用菌中20 种有机磷农药的基质效应[J].亚热带农业研究,2022,18(2):136-141. [19] 党娟. 基质效应对六盘水6 种蔬菜中20 种农药残留检测的影响[J].农技服务,2022,39(6):67-72. [20] 王连珠,王瑞龙,王登飞,等.QuEChERS-LC-MS/MS测定果蔬中氟吡呋喃酮方法优化及基质效应的消除[J].现代食品科技,2020,36(8):347-353.
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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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