Article(id=1153986584132182707, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986579971429187, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20240817001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1723824000000, receivedDateStr=2024-08-17, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1753061441691, onlineDateStr=2025-07-21, pubDate=1740412800000, pubDateStr=2025-02-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1753061441691, onlineIssueDateStr=2025-07-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1753061441691, creator=13701087609, updateTime=1753061441691, updator=13701087609, issue=Issue{id=1153986579971429187, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='4', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='1740412800000', pubDateStr='2025-02-25', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1753061440699, creator='13701087609', updateTime=1758783495950, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1177986619249406427, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986579971429187, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1177986619249406428, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986579971429187, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=97, endPage=103, ext={EN=ArticleExt(id=1153986584794882742, articleId=1153986584132182707, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry, columnId=1153429495274000613, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Research and Detection of Pesticide and Veterinary Drug Residue, runingTitle=null, highlight=null, articleAbstract=
Objective To establish the detection of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were fully dissolved in ultrapure water and extracted by high-speed homogenization of n-hexane, nitrogen blowing and concentration, and purified by QuEChERS method, and the data was collected in selective reaction monitoring mode by GC-MS/MS detection technology, and quantitatively detected by matrix curve and solvent curve. Results The 172 kinds of pesticides had a good linear relationship in the linear range of 10-200 ng/mL, and the linear correlation coefficient was between 0.9962 and 0.9999, the limit of quantification of the method was 0.01 mg/kg, performed 6 repeated spiked experiments at concentrations 1, 2, and 10 times the limit of quantification each, the recovery rate of spikes was between 71.0%-113.0%, and the relative standard deviation (n=6) was 0.49%-17.00%. Conclusion This method can detect hundreds of pesticides in one injection, which is fast, simple, high-throughput and economical, and is suitable for the detection of a variety of pesticide residues in brown sugar.
, authors=null, authorsList=Kun YANG, Mi-Sun HUANG, Xiang-Yu CAI, Jin-Lan QIN, Kai HUANG, Ze-Hua QIN, authorCompany=null, correspAuthors=Ze-Hua QIN, 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=1153986612913496493, articleId=1153986584132182707, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=QuEChERS-气相色谱-串联质谱法测定红糖中172种农药残留, columnId=1153429495479521513, journalTitle=食品安全质量检测学报, columnName=本期专题：农兽药残留研究与检测, runingTitle=null, highlight=null, articleAbstract=
目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)检测红糖中172种农药残留的方法。方法 样品加入超纯水充分溶解后经正己烷高速匀浆提取, 氮吹浓缩, QuEChERS法净化, 采用GC-MS/MS检测技术, 以分段时间选择反应监测模式(selective reaction monitoring, SRM)模式进行数据采集, 配制基质匹配曲线及溶剂曲线进行定量检测。结果 172种农药在10~200 ng/mL质量浓度的线性范围内线性关系良好, 线性相关系数在0.9962~0.9999之间, 定量限为0.01 mg/kg, 在1、2、10倍定量限的浓度下各进行6次重复的加标实验, 平均加标回收率在71.0%~113.0%之间, 相对标准偏差为0.49%~17.00% (n=6)。结论 该方法利用QuEChERS法净化, 一次进样可以检测上百种农药, 具有快速、简便、高通量、经济等特点, 适用于红糖中多种农药残留的检测。
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杨昆(1990—), 女, 硕士, 工程师, 主要研究方向为食品质量与安全。E-mail: 791380766@qq.com
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)])], figs=[ArticleFig(id=1178002226040684674, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=EN, label=Fig.1, caption=
Total ion current map of 208 kinds of pesticide and their metabolites mixed standards in brown sugar (200 ng/mL), figureFileSmall=ksMOKtNF9j3/UHzBfKF20Q==, figureFileBig=GmuZd5VCqzAW2tXdcsGTGQ==, tableContent=null), ArticleFig(id=1178002226141347971, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=CN, label=图1, caption=
红糖中208种农药及其代谢物混合标准品总离子流图(200 ng/mL), figureFileSmall=ksMOKtNF9j3/UHzBfKF20Q==, figureFileBig=GmuZd5VCqzAW2tXdcsGTGQ==, tableContent=null), ArticleFig(id=1178002226212651140, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=EN, label=Fig.2, caption=
Proportion of target compounds that meet the recovery requirements (70%~120%) in different extraction agents, figureFileSmall=egPB9Imqdg5rxpUaZzsP4w==, figureFileBig=P8+tFyECOlyy25Ztiy3hCg==, tableContent=null), ArticleFig(id=1178002226271371397, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=CN, label=图2, caption=
不同提取剂中满足回收率要求(70%~120%)的目标化合物所占比例, figureFileSmall=egPB9Imqdg5rxpUaZzsP4w==, figureFileBig=P8+tFyECOlyy25Ztiy3hCg==, tableContent=null), ArticleFig(id=1178002226342674566, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=EN, label=Fig.3, caption=
Effects of different amounts of GCB and PSA on 172 kinds of target compounds, figureFileSmall=2YhlcJOjmXu1neeguZVrTA==, figureFileBig=iEQxDRysvIZ4NhaugOj0oQ==, tableContent=null), ArticleFig(id=1178002226413977735, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=CN, label=图3, caption=
不同含量GCB和PSA对172种目标化合物的影响, figureFileSmall=2YhlcJOjmXu1neeguZVrTA==, figureFileBig=iEQxDRysvIZ4NhaugOj0oQ==, tableContent=null), ArticleFig(id=1178002226497863816, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=EN, label=Fig.4, caption=
MEs of 172 kinds of compounds in brown sugar, figureFileSmall=WOGAGk3f4s+4neJTEawUlg==, figureFileBig=4Wz2WtkMyL2ZUe/F75aDzw==, tableContent=null), ArticleFig(id=1178002226560778377, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=CN, label=图4, caption=
红糖中172种化合物的MEs, figureFileSmall=WOGAGk3f4s+4neJTEawUlg==, figureFileBig=4Wz2WtkMyL2ZUe/F75aDzw==, tableContent=null), ArticleFig(id=1178002226644664458, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=EN, label=Table 1, caption=
Mass spectrometric parameters and peformance parameters of partial representative pesticides for GC-MS/MS analysis
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 类别 | 中文名 | 保留时间/min | 离子对(m/z) | 碰撞能
/V | r2 | 回收率/% |
| 定量离子 | 定性离子 | 0.01 mg/kg | 0.02 mg/kg | 0.10 mg/kg |
| 1 | 杀虫剂 | 艾氏剂 | 14.9 | 262.7/192.9 | 254.9/220, 262.7/191 | 32,20,30 | 0.9996 | 91.1 (12) | 90.7 (13) | 95.3 (5.2) |
| 2 | 杀虫剂 | 杀螟硫磷 | 14.31 | 277/260 | 125/79, 277/109 | 6,16,6 | 0.9996 | 93.4 (8.6) | 92.9 (5.5) | 97.6 (4.3) |
| 3 | 杀虫剂 | 毒死蜱 | 14.74 | 313.9/257.9 | 196.7/107, 196.7/168 | 12,36,12 | 0.9994 | 91.9 (7.2) | 92.8 (8.6) | 98.3 (3.1) |
| 4 | 杀虫剂 | 对硫磷 | 14.94 | 291/109 | 109/81, 139/109 | 12,10,5 | 0.9993 | 95.2 (5.6) | 96.3 (7.1) | 102 (5.8) |
| 5 | 除草剂 | 甲草胺 | 13.72 | 188.1/160.1 | 160.1/131.7, 188.1/130 | 8,10,32 | 0.9991 | 93.0 (12) | 92.0 (14) | 96.1 (4.2) |
| 6 | 除草剂 | 莠灭净 | 13.89 | 227.1/58.1 | 227.1/170, 227.1/212.1 | 12,10,8 | 0.9994 | 93.8 (7.9) | 92.8 (10) | 94.1 (5.3) |
| 7 | 除草剂 | 二甲戊灵 | 15.66 | 252.1/162 | 252.1/161, 252.1/191.3 | 8,14,8 | 0.9994 | 92.7 (1.9) | 99.6 (6.1) | 92.0 (3.5) |
| 8 | 除草剂 | 丁草胺 | 16.85 | 176.1/146.9 | 188.1/160.1, 236.9/160.1 | 12,10,5 | 0.9994 | 104 (2.8) | 99.6 (3.8) | 99.2 (6.8) |
| 9 | 杀菌剂 | 甲霜灵 | 13.88 | 234/146 | 131.9/117, 160.1/130 | 20,12,18 | 0.9998 | 93.0 (8.9) | 99.9 (9.5) | 105 (4.9) |
| 10 | 杀菌剂 | 苯霜灵 | 19.74 | 148.1/77 | 148.1/79, 148.1/105 | 30,22,20 | 0.9991 | 93.4 (3.2) | 90.3 (5.9) | 95.1 (5.3) |
| 11 | 杀菌剂 | 腐霉利 | 16.23 | 95.9/67.1 | 95.9/53, 283/96.1 | 8,16,8 | 0.9994 | 91.8 (7.3) | 99.2 (4.3) | 94.4 (9.4) |
| 12 | 杀菌剂 | 戊唑醇 | 20.65 | 250/125 | 125/89, 125/99, 250/153 | 20,6,16 | 0.9998 | 92.8 (2.6) | 96.8 (8.1) | 105 (4.3) |
| 13 | 杀螨剂 | 溴螨酯 | 21.89 | 183/155 | 184.9/75.5, 184.9/156.9 | 15,30,12 | 0.9998 | 85.2 (9.2) | 87.2 (17) | 95.5 (4.2) |
| 14 | 杀螨剂 | 乙螨唑 | 22.16 | 140.9/113 | 140.9/62.9, 204/176.1 | 14,26,10 | 0.9998 | 96.0 (8.8) | 99.2 (6.3) | 102 (4.7) |
| 15 | 杀螨剂 | 乙酯杀螨醇 | 18.72 | 139/111 | 139/74.9, 251/139 | 12,26,15 | 0.9992 | 114 (3.2) | 96.0 (7.7) | 96.8 (5.1) |
| 16 | 植物生长调节剂 | 多效唑 | 16.78 | 236/125 | 236/167 | 12,10 | 0.9993 | 92.2 (9.8) | 104 (6.3) | 109 (5.4) |
| 17 | 增效剂 | 增效醚 | 20.98 | 176.1/103.1 | 176.1/117, 176.1/131.1 | 22,18,12 | 0.9993 | 92.8 (6.7) | 96.0 (11) | 96.8 (5.2) |
| 18 | 增效剂 | 溴氰菊酯 | 29.5 | 181/152.1 | 250.7/172, 252.8/92.9 | 22,5,16 | 0.9999 | 102 (5.6) | 92.8 (4.6) | 96.9 (0.45) |
| 19 | 增效剂 | 水胺硫磷 | 15.04 | 136/69 | 121.1/65, 136/108 | 30,14,12 | 0.9997 | 94.1 (11) | 98.4 (6.5) | 104 (5.6) |
), ArticleFig(id=1178002226720161931, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986584132182707, language=CN, label=表1, caption=
GC-MS/MS检测的部分代表性农药残留质谱参数及方法性能参数
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 类别 | 中文名 | 保留时间/min | 离子对(m/z) | 碰撞能
/V | r2 | 回收率/% |
| 定量离子 | 定性离子 | 0.01 mg/kg | 0.02 mg/kg | 0.10 mg/kg |
| 1 | 杀虫剂 | 艾氏剂 | 14.9 | 262.7/192.9 | 254.9/220, 262.7/191 | 32,20,30 | 0.9996 | 91.1 (12) | 90.7 (13) | 95.3 (5.2) |
| 2 | 杀虫剂 | 杀螟硫磷 | 14.31 | 277/260 | 125/79, 277/109 | 6,16,6 | 0.9996 | 93.4 (8.6) | 92.9 (5.5) | 97.6 (4.3) |
| 3 | 杀虫剂 | 毒死蜱 | 14.74 | 313.9/257.9 | 196.7/107, 196.7/168 | 12,36,12 | 0.9994 | 91.9 (7.2) | 92.8 (8.6) | 98.3 (3.1) |
| 4 | 杀虫剂 | 对硫磷 | 14.94 | 291/109 | 109/81, 139/109 | 12,10,5 | 0.9993 | 95.2 (5.6) | 96.3 (7.1) | 102 (5.8) |
| 5 | 除草剂 | 甲草胺 | 13.72 | 188.1/160.1 | 160.1/131.7, 188.1/130 | 8,10,32 | 0.9991 | 93.0 (12) | 92.0 (14) | 96.1 (4.2) |
| 6 | 除草剂 | 莠灭净 | 13.89 | 227.1/58.1 | 227.1/170, 227.1/212.1 | 12,10,8 | 0.9994 | 93.8 (7.9) | 92.8 (10) | 94.1 (5.3) |
| 7 | 除草剂 | 二甲戊灵 | 15.66 | 252.1/162 | 252.1/161, 252.1/191.3 | 8,14,8 | 0.9994 | 92.7 (1.9) | 99.6 (6.1) | 92.0 (3.5) |
| 8 | 除草剂 | 丁草胺 | 16.85 | 176.1/146.9 | 188.1/160.1, 236.9/160.1 | 12,10,5 | 0.9994 | 104 (2.8) | 99.6 (3.8) | 99.2 (6.8) |
| 9 | 杀菌剂 | 甲霜灵 | 13.88 | 234/146 | 131.9/117, 160.1/130 | 20,12,18 | 0.9998 | 93.0 (8.9) | 99.9 (9.5) | 105 (4.9) |
| 10 | 杀菌剂 | 苯霜灵 | 19.74 | 148.1/77 | 148.1/79, 148.1/105 | 30,22,20 | 0.9991 | 93.4 (3.2) | 90.3 (5.9) | 95.1 (5.3) |
| 11 | 杀菌剂 | 腐霉利 | 16.23 | 95.9/67.1 | 95.9/53, 283/96.1 | 8,16,8 | 0.9994 | 91.8 (7.3) | 99.2 (4.3) | 94.4 (9.4) |
| 12 | 杀菌剂 | 戊唑醇 | 20.65 | 250/125 | 125/89, 125/99, 250/153 | 20,6,16 | 0.9998 | 92.8 (2.6) | 96.8 (8.1) | 105 (4.3) |
| 13 | 杀螨剂 | 溴螨酯 | 21.89 | 183/155 | 184.9/75.5, 184.9/156.9 | 15,30,12 | 0.9998 | 85.2 (9.2) | 87.2 (17) | 95.5 (4.2) |
| 14 | 杀螨剂 | 乙螨唑 | 22.16 | 140.9/113 | 140.9/62.9, 204/176.1 | 14,26,10 | 0.9998 | 96.0 (8.8) | 99.2 (6.3) | 102 (4.7) |
| 15 | 杀螨剂 | 乙酯杀螨醇 | 18.72 | 139/111 | 139/74.9, 251/139 | 12,26,15 | 0.9992 | 114 (3.2) | 96.0 (7.7) | 96.8 (5.1) |
| 16 | 植物生长调节剂 | 多效唑 | 16.78 | 236/125 | 236/167 | 12,10 | 0.9993 | 92.2 (9.8) | 104 (6.3) | 109 (5.4) |
| 17 | 增效剂 | 增效醚 | 20.98 | 176.1/103.1 | 176.1/117, 176.1/131.1 | 22,18,12 | 0.9993 | 92.8 (6.7) | 96.0 (11) | 96.8 (5.2) |
| 18 | 增效剂 | 溴氰菊酯 | 29.5 | 181/152.1 | 250.7/172, 252.8/92.9 | 22,5,16 | 0.9999 | 102 (5.6) | 92.8 (4.6) | 96.9 (0.45) |
| 19 | 增效剂 | 水胺硫磷 | 15.04 | 136/69 | 121.1/65, 136/108 | 30,14,12 | 0.9997 | 94.1 (11) | 98.4 (6.5) | 104 (5.6) |
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