UPLC-MS/MS同时测定红糖中9种雌性激素

Simultaneous determination of nine female-steroid hormones in brown sugar by UPLC-MS/MS

建立了红糖中9种雌性激素的超高效液相色谱-串联质谱法测定方法。样品经水溶解后,用乙腈提取,经HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3色谱柱分离,以乙腈-2mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,分别在电喷雾离子源正、负离子模式下以多反应监测模式(MRM)扫描检测,外标法定量分析。结果表明:9种化合物在相应的质量浓度范围内线性良好,相关系数R均大于0.99,检出限为0.2~1.0μg/kg,回收率为92.2%~113.2%,相对标准偏差为1.6%~6.8%。该方法快速、简便、灵敏,适合红糖中激素的检测。

A ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of female-steroid hormones in brown sugar.Brown sugar samples were dissolved in water, and extracted by acetonitrile, then cleaned-up using an HLB column.The analytes were separated on a ACQUITY UPLC HSS T3 column with acetonitrile-water (containing 2 mmol/L ammonium acetate) as mobile phase by gradient elution.The mass spectrometer was detected in multiple reaction monitoring mode(MRM) using positive-ion and negative-ion electrospray ionizations(ESI), respectively.The quantitative analysis was carried out by external standard method.The results showed that the calibration curves had good linearity for 9 female-steroid hormones in the tested concentration ranges, with correlation coefficients of more than 0.99.The average recoveries at three spiked levels were 92.2%~113.2%, and the precisions expressed as relative standard deviations (RSDs) were 1.6%~6.8%.The limits of detection (LOD) were 0.2~1.0 μg/kg.The method proved to be accurate, rapid, sensitive with repeatability and suitable for rapid detection of female hormone in brown sugar.