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  • 冯婉莹,罗浩,黄泽涛.QuEChERS结合UPLC-MS/MS测定菠菜中5种氨基甲酸酯类农药残留[J].食品科学技术学报,2019,37(3):100-104.    [点击复制]
  • FENG Wanying,LUO Hao,HUANG Zetao.Determination of Residues of Five Carbamate Pesticides in Spinach by QuEChERS Coupled with UPLC-MS/MS[J].Journal of Food Science and Technology,2019,37(3):100-104.   [点击复制]
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QuEChERS结合UPLC-MS/MS测定菠菜中5种氨基甲酸酯类农药残留
冯婉莹,罗浩,黄泽涛
0
(广州检验检测认证集团有限公司, 广东 广州 511447)
摘要:
建立了基于QuEChERS技术的超高效液相色谱-串联质谱法(UPLC-MS/MS),对菠菜中的5种氨基甲酸酯类农药残留量进行测定。样品均质后,以乙腈-水(体积比50∶50)提取后,盐析离心,乙腈层用N-丙基乙二胺净化后供UPLC-MS/MS测定。采用电喷雾离子源ESI正离子模式电离,质谱多反应监测模式对目标母离子和子离子进行扫描测定。5种氨基甲酸酯类农药在0.1~20.0μg/L的基质曲线范围内呈良好线性关系,相关系数r大于0.9991,3个水平的平均加标回收率为91.0%~101.0%,方法检出限和定量限分别为0.10~0.20μg/kg和0.25~0.50μg/kg,相对标准偏差为2.15%~5.57%。该方法具有操作简便、快速高效、回收率高、灵敏度高、重复性好等优点,可用于测定菠菜中的5种氨基甲酸酯类农药残留量。
关键词:  超高效液相色谱-串联质谱法  QuEChERS  菠菜  氨基甲酸酯  农药残留
DOI:10.3969/j.issn.2095-6002.2019.03.013
投稿时间:2018-08-02
基金项目:
Determination of Residues of Five Carbamate Pesticides in Spinach by QuEChERS Coupled with UPLC-MS/MS
FENG Wanying,LUO Hao,HUANG Zetao
(Guangzhou Inspection and Testing Certification Group Co, Guangzhou 511447, China)
Abstract:
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC- MS /MS) method for the determination of five carbamate pesticides in spinach was established. Samples were homogenized and extracted by ultrasonic with acetonitrile-water(50∶50 in volume ratio), and then salted out and purified with primary secondary amine sorbent. Under the electrospray ionization (ESI+mode), data of the target parent ions and product ions were collected with mass spectrometric multi-response monitoring scanning detection. The matrix calibration curves of five carbamate pesticides showed the good linearity within the concentrations of 0.1-20.0μg/L with the good correlation coefficient (r>0.9991). The average recoveries of three spiked levels ranged from 91.0%-101.0%, while the limits of detection and limits of quantitation were 0.10-0.20μg/kg and 0.25-0.50μg/kg, respectively. The relative standard deviations were 2.15%-5.57%. This method has good sensitivity and high precision, which is suitable for practical determination of five carbamate pesticides in spinach.
Key words:  UPLC-MS/MS  QuEChERS  spinach  carbamate  pesticide residue