Citation: LI Yinghong, ZHOU Ping, XU Quanhua, ZHAO Huan, SHAO Qiaoyun. Simultaneous determination of seven high risk pesticide residues in royal jelly by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(2): 136-142. doi: 10.3724/SP.J.1123.2017.10012 shu

Simultaneous determination of seven high risk pesticide residues in royal jelly by high performance liquid chromatography-tandem mass spectrometry

1.
Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China;
2.
Hangzhou Beewords Bee Industry Group Co., Ltd., Tonglu 311500, China

Received Date: 15 October 2017

A method was developed for the simultaneous determination of seven high risk pesticides in the royal jelly, eg. tau-fluvalinate, triadimenol, coumaphos, haloxyfop, carbendazim, thiophanate-ethyl and thiophanate-methyl by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). First, the royal jelly samples were extracted with acetonitrile under alkaline conditions. After dehydration by anhydrous sodium sulfate, the extracts were enriched and purified through solid-phase extraction (SPE) with Oasis HLB cartridges. Finally, the pesticides were detected by HPLC-MS/MS method. The separation was carried out on a Venusil MP C18 column with gradient elution. Methanol (containing 0.1% (v/v) formic acid) and 0.5 mmol/L ammonium acetate aqueous solution (containing 0.1% (v/v) formic acid) were used as the mobile phases. The detection was achieved using electrospray ionization in positive ion (ESI⁺) mode and multiple reaction monitoring (MRM) mode for data collection. Quantification was carried out using internal standard method. The results showed that the seven high risk pesticides were linear in the range of 5-100 μg/kg. The linear correlation coefficients (r²) were 0.9921-0.9996. The limits of detection (LODs) and limits of quantification (LOQs) of the seven high risk pesticides were 0.5-2.0 μg/kg and 1.0-5.0 μg/kg, respectively. The average recoveries at the three spiked levels were 80.5%-101.3%, and the relative standard deviations were 3.6%-9.4% (n=3). This method is simple, effective and sensitive, and is suitable for the determination of the pesticide residues in royal jelly.
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沈阳化工大学材料科学与工程学院沈阳 110142