色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 741-745.DOI: 10.3724/SP.J.1123.2014.01043

• 研究论文 • 上一篇    下一篇

气相色谱-负化学源质谱法测定蜂蜜和王浆中4种杀虫剂的残留

夏广辉1, 沈伟健2, 余可垚2, 吴斌2, 张睿2, 沈崇钰2, 赵增运2, 卞筱泓1, 许激扬1   

  1. 1. 中国药科大学生物化学教研室, 江苏 南京 210009;
    2. 江苏出入境检验检疫局食品实验室, 江苏 南京 210001
  • 收稿日期:2014-01-26 修回日期:2014-05-05 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 许激扬，E-mail：jiyang_xu@sina.cn.
  • 基金资助:

    国家质检总局科技计划项目（2011KJ39，2012KJ31，2012IK167）.

Determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry

XIA Guanghui1, SHEN Weijian2, YU Keyao2, WU Bin2, ZHANG Rui2, SHEN Chongyu2, ZHAO Zengyun2, BIAN Xiaohong1, XU Jiyang1   

  1. 1. Department of Biochemistry, China Pharmaceutical University, Nanjing 210009, China;
    2. Food Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2014-01-26 Revised:2014-05-05 Online:2014-07-08 Published:2014-06-25

PDF

221

被引次数

10

摘要：

建立了气相色谱-负化学源质谱（GC-NCI/MS）测定蜂蜜和王浆中4种杀虫剂残留量的方法。蜂蜜样品由乙酸乙酯提取、乙二胺-N-丙基硅烷（PSA）净化，而王浆样品经乙腈-水（1：1，v/v）提取、C18固相萃取柱净化，采用GC-NCI/MS测定，外标法定量。结果表明：在50~500 μg/L范围内4种农药的线性良好；所有农药的LOD在0.12~5.0 μg/kg之间，LOQ在0.40~16.5 μg/kg之间；在10、15、20 μg/kg 3个添加水平下，4种农药的平均回收率在78.2%~110.0%之间，且RSD均小于14%。所有农药的测定均没有出现干扰峰。该方法简单、快速，准确度、精密度和选择性高，抗干扰能力强，可用于蜂蜜和王浆中这4种农药的快速检测。

关键词: 蜂蜜, 气相色谱-负化学源质谱, 杀虫剂, 王浆

Abstract:

A method was developed for the determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The honey and royal jelly samples were treated with different preparation methods as the result of the different components. The honey sample was extracted with ethyl acetate and cleaned up with primary second amine, and the royal jelly sample was extracted with acetonitrile-water (1:1, v/v), and cleaned up with a C18 solid-phase extraction column. Finally, the extracts of the honey and royal jelly were analyzed by GC-NCI/MS in selected ion monitoring (SIM) mode separately. External standard calibration method was used for quantification. The linearities of calibration curves of the four insecticides were good with the correlation coefficients greater than 0.99 in the range of 50-500 μg/L. The limits of the detection (LODs) of the four insecticides were in the range of 0.12-5.0 μg/kg, and the limits of the quantification (LOQs) were in the range of 0.40-16.5 μg/kg. The recoveries of the four insecticides spiked in honey and royal jelly at three spiked levels (10, 15 and 20 μg/kg) were in the range of 78.2%-110.0%, and the relative standard deviations (RSDs) were all below 14%. The sensitivity and selectivity of this method were good with no interfering peaks. The proposed method is simple, quick and effective to analyze the four insecticide residues in honey and royal jelly.

Key words: gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS), honey, insecticides, royal jelly

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