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目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测红糖中雌二醇的分析方法。方法红糖样品用乙腈提取,经QuEChERS方法净化后,采用HPLC-MS/MS进行分析检测,在电喷雾质谱负离子模式(ESI~-),多反应监测(MRM)模式检测,同位素内标法定量。结果该方法在1~50μg/L范围内线性良好(r=0.9996),检出限为0.7μg/kg。分别在样品中添加雌二醇标准溶液2、5、10μg/kg水平上进行添加回收率实验,方法的回收率范围为101%~114%,相对标准偏差为2.2%~4.9%(n=6)。结论该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度满足红糖中雌二醇的检测要求。
Objective To establish a method for the determination of estradiol in brown sugar by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods The brown sugar samples were extracted with acetonitrile and purified by QuEChERS method. The samples were analyzed by HPLC-MS / MS and detected by electrospray mass spectrometry negative ion mode (ESI ~ -), multiple reaction monitoring (MRM) mode and isotope internal standard method. Results The method was linear in the range of 1 ~ 50 μg / L (r = 0.9996) with a detection limit of 0.7 μg / kg. The recoveries of spiked samples at the spiked levels of 2, 5, and 10 μg / kg of estradiol standard solutions were determined. The recoveries ranged from 101% to 114% with relative standard deviations of 2.2% to 4.9% (n = 6 ). Conclusion The method of sample preparation is simple and rapid, the analysis time is short, and the sensitivity, accuracy and precision meet the detection requirements of estradiol in brown sugar.