液相色谱-串联质谱法测定化妆品中多种激素

Determination of various hormones in cosmetics by liquid chromatography together with mass spectrometry

采用液相色谱-串联质谱法测定化妆品中糖皮质激素、雌激素、雄激素、孕激素等激素的含量。不同形态的化妆品样品以甲醇为提取剂进行超声提取,样品提取液离心后得到上清液经HLB固相萃取小柱净化,用Agilent ZORBAXEclipse XDB-C18柱(1.8μm,2.1 mm×50 mm),乙腈-水作为流动相,梯度洗脱,流速0.3 mL/min,柱温25℃,进样量2.0μL,糖皮质激素、雄激素、孕激素采用正离子扫描模式,雌激素采用负离子扫描模式,多反应监测测定。化妆品样品平均加标回收率为72.31%~97.89%,相对标准偏差为2.24%~11.34%,方法检出限为0.002 mg/kg^0.8 mg/kg。

Content of various kinds of hormones, including glucocorticoids, oestrogens, androgens and progestogen in cosmetics were determined by liquid chromatography together with mass spectrometry. Various cosmetics samples were extracted by methyl alcohol under help of ultrasonic wave. The extracts were centrifuged , and the upper clear solutions were purified by HLB SPE columns and separated with Agilent ZORBAX Eclipse XDB - C18 column （ 1. 8μm, 2. 1 mm × 50 mm ）, using a mobile phase consist of acetonitrile - water and gradient eluted at a flow rate of 0.3 mL/min. The column temperature was 25℃ and the injection volume was 2.0 μL. Glucocorticoids, androgens and progestogen were analyzed in the positive ion scanning mode,while oestrogens were analyzed in the negative ion scanning mode. The detections were made with MRM mode. The average recoveries achieve between 72.31% and 97.89%, and the relative standard deviations （RSD） achieve between 2. 24% and 11. 34%. The detection limits of this method achieves 0. 002 mg/kg - 0.8 mg/kg.