Citation: XIA Guanghui, SHEN Weijian, YU Keyao, WU Bin, ZHANG Rui, SHEN Chongyu, ZHAO Zengyun, BIAN Xiaohong, XU Jiyang. Determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(7): 741-745. doi: 10.3724/SP.J.1123.2014.01043 shu

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

1.
1. Department of Biochemistry, China Pharmaceutical University, Nanjing 210009, China;

Corresponding author: XU Jiyang,
Received Date: 26 January 2014
Available Online: 5 May 2014
Fund Project: 国家质检总局科技计划项目(2011KJ39,2012KJ31,2012IK167). (2011KJ39,2012KJ31,2012IK167)

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