1. 重庆医科大学药学院
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
3. 中国检验检疫科学研究院
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何小琴, 郗存显, 唐柏彬, 等. 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[J]. 分析测试学报, 2014,33(6):635-641.
Rapid Determination of Illegally Added 25 Hormones in Oral by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2014,33(6):635-641.
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-ODS Ⅱ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0.5~50 μg/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0.099~0.492 μg/kg,检出限为0.029~0.147 μg/kg。在0.5,1.0,5.0 μg/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 from 0.029 μg/kg to 0.147 μg/kg and the limits of quantitation(LOQ) ranged from 0.099 μg/kg to 0.492 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.
口服液激素超高效液相色谱-串联质谱法(UPLC-MS/MS)
oralhormoneultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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