超高效液相色谱-串联质谱法快速测定口服液中非法添加的25种激素  

Rapid Determination of Illegally Added 25 Hormones in Oral by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：何小琴[1] 郗存显[2] 唐柏彬[2] 王国民[2] 彭涛[3] 陈冬东[3] 母昭德[1] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆出入境检验检疫局重庆市进出口食品安全工程技术研究中心,重庆400020 [3]中国检验检疫科学研究院,北京100123

出　　处：《分析测试学报》2014年第6期635-641,共7页Journal of Instrumental Analysis

基　　金：“十二五”科技支撑计划项目(2012BAD33B02)

摘　　要：建立了快速检测延缓衰老口服液中9种孕激素、7种雄激素、7种糖皮质激素及2种雌激素的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。样品经1%乙酸-乙腈溶液、甲醇分步提取,浓缩至干后,用甲醇-水（1∶1）溶解残渣,Shim-pack XR-ODSⅡ色谱柱梯度分离,采用电喷雾正离子模式电离,基质匹配标准曲线定量。结果表明：25种化合物在0.5～50μg/L范围内呈良好的线性关系,相关系数均大于0.99,定量下限为0.099～0.492μg/kg,检出限为0.029～0.147μg/kg。在0.5,1.0,5.0μg/kg 3个加标水平下,各化合物的平均回收率为73.3%～122.2%,相对标准偏差（RSD）为5.1%～14.9%。该方法简便、快速、准确,适用于延缓衰老口服液中多种激素的同时、快速测定。A sensitive ultra performance liquid chromatography-tandem mass spectrometric（ UPLC-MS /MS） method was developed for the simultaneous determination of 9 progesterones,7 androgens,7 glucocorticoids,2 estrogens in anti-aging oral samples. The analytes were stepwise extracted with acetonitrile containing 1% acetic acid and methanol,the extract was concentrated to dryness,redissolved in methanol-water（ 1 ∶ 1）. 25 hormones were gradient separated on a Shim-pack XR-ODS Ⅱ column,and analyzed by electrospray ionization under positive ion mode with matrix standard curve. As a result,the calibration curves for all target compounds were linear in the range of 0. 5-50 μg /L with correlation coefficients larger than 0. 99. The limits of detection（ LOD） ranged from0. 029 μg /kg to 0. 147 μg /kg and the limits of quantitation（ LOQ） ranged from 0. 099 μg /kg to0. 492 μg /kg. The average recoveries of 25 compounds at spiked levels of 0. 5,1. 0,5. 0 μg /kg were in the range of 73. 3%-122. 2% with relative standard deviations（ RSD） of 5. 1%-14. 9%.The method is simple,rapid and accurate,and is suitable for the rapid determination of hormones in anti-aging function foods.

关 键 词：口服液 激素 超高效液相色谱-串联质谱法(UPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学] O629.8[理学—化学]