超高效液相色谱-大气压化学电离-三重四极杆质谱法同时测定保健食品中14种性激素类药物

doi:10.3724/SP.J.1123.2018.12039

色谱 ›› 2019, Vol. 37 ›› Issue (6): 626-633.DOI: 10.3724/SP.J.1123.2018.12039

超高效液相色谱-大气压化学电离-三重四极杆质谱法同时测定保健食品中14种性激素类药物

饶雅琨, 李卓, 张荻悦, 董曼曼, 卫星华, 陈冬, 张亚锋

西安市食品药品检验所, 陕西西安 710054

收稿日期:2018-12-27 出版日期:2019-06-08 发布日期:2015-04-17
通讯作者: 张亚锋,Tel:(029)85520126,E-mail:27327242@qq.com.
基金资助:
陕西省科技厅重点研发计划（2017SF-311）；西安市碑林区应用技术研发项目（GX1706）.

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

RAO Yakun, LI Zhuo, ZHANG Diyue, DONG Manman, WEI Xinghua, CHEN Dong, ZHANG Yafeng

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

Received:2018-12-27 Online:2019-06-08 Published:2015-04-17
Supported by:
Key Research and Development Plan of Shaanxi Science & Technology Department (No. 2017F-311); Xi'an Municipal Science & Technology Bureau Beilin District Technology Research and Development Project (No. GX1706).

摘要/Abstract

摘要：

建立了超高效液相色谱-大气压化学电离-三重四极杆质谱（UPLC-APCI-MS/MS）测定保健食品中14种性激素类药物的方法。样品用乙腈提取2次，再用HLB固相萃取柱净化处理。采用Hypersil Gold C18色谱柱（100 mm×2.1 mm，1.9 μm）分离，以乙腈-10 mmol/L乙酸铵溶液为流动相进行梯度洗脱，采用APCI-三重四极杆质谱检测，外标法定量。结果表明，14种性激素类药物在各自范围内线性关系良好，相关系数（r）≥0.996，检出限为0.0990~2.09 μg/kg，定量限为0.495~5.23 μg/kg；在低、中、高3个水平下的平均加标回收率为65.8%~118.8%，精密度为0.6%~8.7%（n=6）。该方法前处理简单，灵敏度高，回收率良好，适用于保健食品中性激素类非法添加物的定量测定。

关键词: 保健食品, 超高效液相色谱-三重四极杆质谱, 大气压化学电离, 性激素类药物

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.

Key words: atmospheric pressure chemical ionization (APCI), health care products, sexual hormones, ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

饶雅琨, 李卓, 张荻悦, 董曼曼, 卫星华, 陈冬, 张亚锋. 超高效液相色谱-大气压化学电离-三重四极杆质谱法同时测定保健食品中14种性激素类药物[J]. 色谱, 2019, 37(6): 626-633.

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.

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超高效液相色谱-大气压化学电离-三重四极杆质谱法同时测定保健食品中14种性激素类药物

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

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