超高效液相色谱串联质谱法对饮料中6种雌激素的测定

Determination of six Estrogens in Beverages by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

目的:建立一种高效快速检测饮料中雌二醇、雌三醇、雌酮、己烯雌酚、己二烯雌酚和己烷雌酚等6种雌激素的超高效液相色谱串联质谱法。方法:选取三种具有代表性的饮料基质,加入乙腈和QuEChERS萃取包提取2次,合并提取液,50℃氮吹至干,残渣用甲醇一0.5%氨水(体积比9∶1)溶解。以甲醇和0.5%氨水溶液为流动相,使用C18色谱柱进行分离,以LC-MS/MS多反应监测模式开展定性及定量分析,外标法定量。结果:结果表明,方法检出限为0.3μg/kg~3.0μg/kg。在添加水平为10μg/kg~100μg/kg范围内的平均回收率为72.5%~119%,相对标准偏差为6.7%~11.4%。本方法灵敏度高、前处理快捷高效,适用于饮料中6种雌激素的检测与定量分析。

Objective:To establish an efficient and rapid ultra-high performance liquid chromatography tandem mass spectrometry method for the detection of estradiol,estradiol,estrone,dienestrol,diethylstilbestrol and hexestrol in beverages.Methods:Three representative beverage substrates were selected and extracted with acetonitrile and QuEChERS extraction kit two times,combined with the extraction solution,nitrogen was blown to dry at 50℃,and the residue was dissolved with methanol to 0.5%ammonia water(volume ratio 9∶1).Methanol and 0.5%ammonia solution were separated by C18 column.Qualitative and quantitative analysis were carried out by LC-MS/MS multi-reaction monitoring mode.Quantitative analysis was carried out by external standard method.Result:The results showed that the detection limit of the method was 0.3μg/kg~3.0μg/kg.The average recovery was 72.5%to 119%and the relative standard deviation was 6.7%to 11.4%in the range of 10μg/kg~100μg/kg.The method has high sensitivity,fast and efficient pretreatment,and is suitable for the detection and quantitative analysis of 6 estrogen in beverages.