Citation: RAO Yakun, LI Zhuo, ZHANG Diyue, DONG Manman, WEI Xinghua, CHEN Dong, ZHANG Yafeng. Simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(6): 626-633. doi: 10.3724/SP.J.1123.2018.12039 shu

Simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry

Xi'an Institute for Food and Drug Control, Xi'an 710054, China

Received Date: 27 December 2018

Fund Project: Key Research and Development Plan of Shaanxi Science & Technology Department (No. 2017F-311)

A comprehensive analytical method was developed for the simultaneous determination of 14 sexual hormones in health care products by ultra performance liquid chromatography-atmospheric pressure chemical ionization-triple quadrupole mass spectrometry (UPLC-APCI-MS/MS). The samples were extracted twice with acetonitrile and the extracts were purified using hydrophilic-lipophilic balance (HLB) cartridges. Chromatographic separation was achieved on a Hypersil Gold C18 column (100 mm×2.1 mm, 1.9 μm) by gradient elution with acetonitrile and 10 mmol/L ammonium acetate aqueous solution as the mobile phases. Compounds were detected by APCI-MS/MS with external standard calibration curve method. All the 14 sexual hormones showed a good linear trend in their respective concentration ranges and the correlation coefficients (r) were no less than 0.996. The limits of detection (LODs) ranged from 0.0990 μg/kg to 2.09 μg/kg. The limits of quantification (LOQs) were in the range of 0.495-5.23 μg/kg. The average recoveries of the 14 sexual hormones in the health care product samples ranged from 65.8% to 118.8% at the three spiked levels. The precisions (n=6) ranged from 0.6% to 8.7% (n=6). The method is simple, sensitive, accurate and precise, and is suitable for the determination of the illegal added sexual hormones in the health care products.
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