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

Abstract

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.