固相萃取-超高效液相色谱-串联质谱法测定水中6种雌激素  

Determination of Six Estrogens in Water Using Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：赵云芝[1] 钱蜀 谢永洪[1] 郑昌结 杨秋红[1] 

机构地区：[1]四川省环境监测中心站,四川成都610041

出　　处：《中国环境监测》2013年第1期107-111,共5页Environmental Monitoring in China

摘　　要：建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS-MS)同时检测水样中6种雌激素(壬基酚、双酚A、雌酮、17α-雌二醇、17α-乙炔雌二醇、雌三醇)的方法。样品采用SPE小柱富集后,用90%乙腈-0.1%氨水混合溶液洗脱浓缩定容。在梯度洗脱条件下,6种雌激素用三重四极杆串联质谱检测。该方法显示出良好的线性关系(r>0.999)和精密度(RSD<10%),方法检出限为1.3～5.2 ng/L。该方法成功应用于地表水、地下水和废水样品中6种雌激素分析,样品加标回收率为76.8%～117%。该方法准确、灵敏、无需衍生,可用于同时测定水样中的6种雌激素。A method using solid pahase extraction-ultra performance liquid chromatography-tandem mass spectrometry （SPE- UPLC-MS-MS） for the simultaneous determination of 6 estrogens （Nonylphenol, Bisphenol A, Estrone, 17a-Estradiol, 17ct- Ethinylestradiol, Estriol） in water was developed. After the sample was enriched by spe column, it was eluted by 90% acetonitrile-0.1% ammonia solution and then condensed and constant volume. Under gradient elution, six estrogens were detected by tandem mass spectrometry, it shows good linearity （r 〉 0. 999）and precision （RSD 〈 10% ）. the method detection limit for six estrogens ranged from 1.3 ng/L to 6.9 ng/L. It had been successfully applied to the analysis of six estrogens in surface water,underground water and waste water. The spiked recoveries of samples were in the range of 76. 8%-117%. The method is simple and accurate for simultaneously analyzing the six estrogens in water.

关 键 词：固相萃取 超高效液相色谱-串联质谱 雌激素 水样 

分 类 号：X830.2[环境科学与工程—环境工程]