高效液相色谱-串联质谱法测定红糖中雌二醇

Determination of estradiol in brown sugar by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  红糖  雌二醇  QuEChERS  高效液相色谱串联质谱法

英文关键词:brown sugar  estradiol  QuEChERS  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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1~50 μg/L范围内线性良好(r=0.9996), 检出限为0.7 μg/kg。分别在样品中添加雌二醇标准溶液2、5、10 μg/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。

英文摘要:

      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 sugar samples were extracted by acetonitrile, cleaned up by developed QuEChERS method, and then analyzed by HPLC-MS/MS in multiple reaction monitoring (MRM) mode via negative electrospray ionization (ESI-). Isotope internal standards were used for quantitative analysis. Results External standard method was used to determine the estradiol contents with a good linear relationship in the range of 1~50 μg/L (r=0.9996). The limit of quantification (LOQ) was 0.7 μg/kg. The recoveries of estradiol at three levels of 2, 5, and 10 μg/kg were from 101% to 114% with the relative standard deviations (RSDs) of 2.2%~4.9% (n=6) in brown sugar. Conclusion The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the determination of estradiol in brown sugar.