G/CM/SMS法同时测定海产品中4种雌激素残留  

Determination of estrogens in marine foods by gas chromatography/mass/mass spectrometry

作　　者：王玉飞[1] 周凯[1] 李继革[1] 

机构地区：[1]浙江省宁波市疾病预防控制中心,浙江宁波315010

出　　处：《中国卫生检验杂志》2006年第1期21-23,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立海产品中己烯雌酚（DES）、雌酮（E1）、雌二醇（E2）、雌三醇（E3）的GC／MS和GC／MS／MS分析方法。方法：以氯仿-水为提取溶剂，经均质、超声、石油醚去脂、C18固相小柱净化处理，目标物用N，O-双（三甲基硅烷基）三氟乙酰胺衍牛化后，用GC／MS和GC／MS／MS方法分析。结果：4种雌激素的平均回收率在75％～96．7％之间，GC／MS方法榆出限为0．15～0．50μg／kg，方法相对标准偏差为3．32％-5.54％；GC／MS／MS方法检出限为0．05—0．15μg／kg，方法相对标准偏差为6．1％～10．3％。结论：GC／MS／MS方法灵敏度高、特异性强、检出限低、定性确证性强，适用于海产品中4种雌激素残留的微量分析。Objective：To develop a new method for the simultaneous determination of diethylstilbestrol（ DES）, estrone（ E1 ）, estradiol（E2） and estriol（E3） in shrimp, crayfish,crab by GC/MS and GC/MS/MS. Methods： Estrogens was extracted with methylene chloride and water（ 3：1 ） followed by homogenizing and ultrasonic procedure. After clean - up by a C18 SPE column procedure, the target chemicals was derivatized with N, O -bis（trimethylsilyl） -trifluoroaeetamide and separated, detected, confirmed by GC/MS and GC/MS/MS. Results： Good linearity of the calibration curve was obtained in the concentration range from 0. 1 mg/L to 2 mg/L The recoveries for these compounds from shrimp was 75% to 96. 7%. The relative standard deviation was 3. 32% to 5.54% ,the detection limits of the method ranged from 0. 15μg/kg to 0. 50 Ixg/kg by GC/MS and 6. 1% - 10. 3%, 0.05 Ixg/kg to 0. 15μg/kg by GC/MS/MS respectively. Estrogens can be quantitated and confirmed at 0.1 μg/kg level. The results are accurate and reproducible in very complex matrix.

关 键 词：海产品 雌激素 GC/MS GC/MS/MS 

分 类 号：O657.63[理学—分析化学]