通过式固相萃取-超高效合相色谱-串联质谱法测定保健食品中19 种性激素

doi:10.7506/spkx1002-6630-20210824-314

食品科学 ›› 2022, Vol. 43 ›› Issue (20): 370-376.doi: 10.7506/spkx1002-6630-20210824-314

• 安全检测 • 上一篇

通过式固相萃取-超高效合相色谱-串联质谱法测定保健食品中19 种性激素

杨光勇，梁秋艳，阳胜，罗岩，宋敏，袁辉

（新疆维吾尔自治区产品质量监督检验研究院，新疆乌鲁木齐 830011）

出版日期:2022-10-25 发布日期:2022-10-26
基金资助:
新疆维吾尔自治区市场监督管理局科技项目（202102）

Determination of 19 Sex Hormones in Health Foods by Ultra Performance Convergence Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction

YANG Guangyong, LIANG Qiuyan, YANG Sheng, LUO Yan, SONG Min, YUAN Hui

(Xinjiang Product Quality Supervision and Inspection Research Institute, ürümqi 830011, China)

Online:2022-10-25 Published:2022-10-26

摘要/Abstract

摘要： 建立超高效合相色谱-串联质谱测定保健食品中19 种性激素含量的方法。样品经体积分数1%甲酸-甲醇溶液提取、PRiME HLB通过式固相萃取柱净化后，以UPCC Torus 2-PIC色谱柱（3.0 mm×100 mm，1.7 μm）为分析柱，以超临界CO2和体积分数0.1%甲酸-甲醇溶液为流动相梯度洗脱，分别以97%甲醇溶液（含体积分数0.2%甲酸）和98%乙腈溶液（含体积分数0.2%氨水）为补偿液，用配备电喷雾电离源的三重四极杆质谱在正负离子同时扫描、多反应监测模式下测定，外标法定量。结果表明：19 种性激素在各自范围内线性关系良好（R2≥0.997 1），检出限为0.03～0.85 μg/kg（RSN＝3），定量限为0.10～2.5 μg/kg（RSN＝10）；在3 个加标水平下的平均回收率为77.8%～111.7%（n＝9），相对标准偏差为1.1%～8.4%。利用该方法可用于对实际样品进行检测。该方法简便快速、灵敏度高、专属性好、绿色环保，可用于测定保健食品中多种性激素的含量。

关键词: 通过式固相萃取；超高效合相色谱-串联质谱；性激素；保健食品

Abstract: A method based on ultra performance convergence chromatography-tandem mass spectrometry (UPCC-MS/MS) with pass-through solid phase extraction was established for the determination of 19 sex hormones in health foods. The samples were extracted with methanol containing 1% formic acid, and the extract was purified by solid phase extraction using PRiME HLB columns. The chromatographic separation was achieved on a UPCC Torus 2-PIC column (3.0 mm × 100 mm, 1.7 μm) under gradient elution using a mobile phase composed of supercritical carbon dioxide and methanol containing 0.1% formic acid. The separated compounds were analyzed by tandem MS with an electrospray ionization (ESI) source in the positive/negative alternate mode using multiple reaction monitoring. Ninety-seven percent methanol containing 0.2% formic acid and 98% aqueous acetonitrile containing 0.2% ammonia water were used as the auxiliary pump mobile phases. The external standard method was used to quantitatively analyze the sex hormones in sample solutions. Good linear relationship was obtained between the peak area and concentration in the tested concentration ranges (R2 ≥ 0.997 1). The limits of detection and limits of quantification were 0.03?0.85 (RSN = 3) and 0.10?2.5 μg/kg (RSN =10), respectively. The average recoveries (n = 9) at three spiked levels were in the range of 77.8%?111.7% with relative standard deviations (RSDs) between 1.1% and 8.4%. The developed method was successfully used for the determination of actual samples. This method is fast, simple, specific, environmentally friendly and suitable to determine the contents of sex hormones in health foods.

Key words: pass-through solid phase extraction; ultra performance convergence chromatography-tandem mass spectrometry; sex hormones; health foods

中图分类号:

O657.63

杨光勇，梁秋艳，阳胜，罗岩，宋敏，袁辉. 通过式固相萃取-超高效合相色谱-串联质谱法测定保健食品中19 种性激素[J]. 食品科学, 2022, 43(20): 370-376.

YANG Guangyong, LIANG Qiuyan, YANG Sheng, LUO Yan, SONG Min, YUAN Hui. Determination of 19 Sex Hormones in Health Foods by Ultra Performance Convergence Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction[J]. FOOD SCIENCE, 2022, 43(20): 370-376.

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通过式固相萃取-超高效合相色谱-串联质谱法测定保健食品中19 种性激素

Determination of 19 Sex Hormones in Health Foods by Ultra Performance Convergence Chromatography-Tandem Mass Spectrometry with Pass-through Solid Phase Extraction

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