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1.海南省检验检测研究院食品检验检测中心 国家市场监督管理总局重点实验室(热带果蔬质量与安全),海南 海口 570314
2.中国热带农业科学院分析测试中心 海南省热带果蔬产品质量安全重点实验室, 海南 海口 571101
刘春华,硕士,副研究员,研究方向:农产品质量与安全,E-mail:chunhualiu111@126.com
李春丽,硕士,副研究员,研究方向:农产品质量与安全,E-mail:lichunli0111@163.com
收稿日期:2024-11-21,
修回日期:2025-01-26,
录用日期:2025-03-03,
纸质出版日期:2025-07-15
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潘永波,赵静,万娜,刘春华,李春丽.改进的QuEChERS/液相色谱-质谱联用法测定椰汁饮料中90种农药及其代谢物残留量[J].分析测试学报,2025,44(07):1338-1345.
PAN Yong-bo,ZHAO Jing,WAN Na,LIU Chun-hua,LI Chun-li.Determination of 90 Pesticide and Their Metabolites Residues in Coconut Meat Juice by Modified QuEChERS/LC-MS/MS Method[J].Journal of Instrumental Analysis,2025,44(07):1338-1345.
潘永波,赵静,万娜,刘春华,李春丽.改进的QuEChERS/液相色谱-质谱联用法测定椰汁饮料中90种农药及其代谢物残留量[J].分析测试学报,2025,44(07):1338-1345. DOI: 10.12452/j.fxcsxb.241121550.
PAN Yong-bo,ZHAO Jing,WAN Na,LIU Chun-hua,LI Chun-li.Determination of 90 Pesticide and Their Metabolites Residues in Coconut Meat Juice by Modified QuEChERS/LC-MS/MS Method[J].Journal of Instrumental Analysis,2025,44(07):1338-1345. DOI: 10.12452/j.fxcsxb.241121550.
建立了椰汁饮料中90种农药及其代谢物的液相色谱-质谱联用(LC-MS/MS)分析方法。椰汁饮料样品经1%(体积分数)甲酸乙腈提取,使用N-丙基乙二胺(PSA)、脂肪和蛋白质吸附剂(LPAS)、弗罗里硅土(Florisil)、氨基化-多壁碳纳米管(NH
2
-MWCNTs)净化材料,改进的QuEChERS前处理方法对样品提取液进行净化,多反应监测(MRM)模式分析,基质匹配标准曲线外标法定量。结果表明:90种农药及其代谢物在0.002~0.2 mg/L范围内具有良好的线性关系,相关系数(
r
2
)均大于0.99,定量下限(LOQ)均为0.01 mg/kg,在低、中、高3个加标水平下的平均回收率为60.6%~118%,相对标准偏差(RSD)为0.60%~12%(
n=
6)。该方法净化效果好,操作简单,适用于椰汁饮料中多种农药残留的检测。
A method for the determination of 90 pesticides and their metabolites residues in coconut m
eat juice was established by liquid chromatography-tandem mass spectrometry(LC-MS/MS). The coconut meat juice samples were extracted with 1% formic acid acetonitrile,purified by dispersive solid phase extraction columns containing N-propylethylenediamine(PSA),lipid and protein adsorbent (LPAS),Florisil and aminated-multi-walled carbon nanotubes(NH
2
-MWCNTs) purification materials,analyzed by multi-reaction monitoring (MRM) mode,and quantified by external standard method of matrix-matched standard curve. The results showed that the 90 pesticides and their metabolites showed good linearity in the range of 0.002-0.2 mg/L with the correlation coefficients(
r
2
) more than 0.99,and the limit of quantification(LOQ) was 0.01 mg/kg. Average recoveries at three spiked levels were 60.6%-118% with relative standard deviations(RSDs) of 0.60%-12% (
n=
6). This method has good purification effect and simple operation. It is suitable for the determination of various pesticide residues in coconut meat juice.
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