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《化学分析计量》 2019年第03期
DOI:10.3969/j.issn.1008-6145.2019.03.002
高效液相色谱-串联质谱法测定保健食品中20 种雌性激素
罗文静,梁媛,周智明,刘小玉
广东省药品检验所,广州 510663 
Determination of 20 estrogens in health foods by high performance liquid chromatography-tandem mass spectrometry
LUO Wenjing, LIANG Yuan, ZHOU Zhiming, LIU Xiaoyu
Guangdong Drug Inspection Institute, Guangzhou 510663, China 
摘要:建立高效液相色谱-串联质谱法同时测定保健食品中20 种雌性激素的含量。样品用甲醇超声提取后, 经Thermo RP-MS 色谱柱(100 mm×2.1 mm,2.6 μm)分离,雌三醇等9 种激素采用ESI 源负离子模式,苯甲酸雌二醇等11 种激素采用ESI 源正离子模式电离,用多反应监测模式进行定性和定量分析。19 种雌性激素的质量浓度在0.04~2.0 μg/mL,己烯雌酚的质量浓度在0.01~0.7 μg/mL 与色谱峰面积呈良好的线性关系,相关系数均大于0.995,方法检出限为0.01~0.04 mg/kg。在3 个不同浓度加标水平下,平均回收率为80.3%~114.5%,测定结果的相对标准偏差为2.2%~5.8%。该方法灵敏度高,专属性强,适用于保健食品中雌性激素的检测分析。 
Abstract:A method for simultaneous determination of 20 estrogens in health foods by high performance liquid chromatography-tandem mass spectrometry was established. Samples were extracted by methanol ultrasound and separated by Thermo RP-MS column (100 mm×2.1 mm, 2.6 μm). Nine hormones such as estriol were ionized by ESI source negative ion mode and eleven hormones such as estradiol benzoate were ionized by ESI source positive ion mode. The multi-reaction monitoring model was used for qualitative and quantitative analysis. The mass concentration of 19 estrogens in the range of 0.04-2.0 μg/mL, and the mass concentration of diethylstilbestrol in the range of 0.01-0.7 μg/mL, had good linear relationship with the hromatographic peak area, the correlation coefficients were all more than 0.995, and the detection limit of the method was 0.01-0.04 mg/kg. The average recovery rate was 80.3 %-114.5 % at three different concentration levels, and the relative standard deviation of the determination results were 2.2%-5.8%. The method has high sensitivity and specificity, and is suitable for the detection and analysis of estrogen in health food. 
关键词:保健食品;高效液相色谱-串联质谱法;雌性激素 
Keywords:health food; high performance liquid chromatography-tandem mass spectrometry; estrogen 
基金:广东省中医药局科研项目(No.20191041) 
本文引用格式:
罗文静,梁媛,周智明,等. 高效液相色谱- 串联质谱法测定保健食品中20 种雌性激素[J]. 化学分析计量,2019,28(3):5-8.
LUO W J,LIANG Y,ZHOU Z M,et al. Determination of 20 estrogens in health foods by high performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2019,28(3):5-8. 

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