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

作　　者：高裕锋[1] 甄振鹏[1] 张琳[1] 余构彬[1] 郭剑雄[1] 李海乔[1] 

机构地区：[1]广州甘蔗糖业研究所,广东省甘蔗改良与生物炼制重点实验室,国家糖业质量监督检验中心,广州510316

出　　处：《食品安全质量检测学报》2016年第9期3465-3469,共5页Journal of Food Safety and Quality

基　　金：广东省科技计划项目(2013B040400003,2013B061800023,2013B061800007,2014B040404054,2016A040403066)

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1~50μg/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 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.

关 键 词：红糖 雌二醇 QUECHERS 高效液相色谱串联质谱法 

分 类 号：O657.63[理学—分析化学] TS247[理学—化学]