全自动固相萃取-气相色谱-质谱法测定水中6种苯氧羧酸类除草剂  

Determination of 6 phenoxycarboxylic acid herbicides in drinking water by automatic solid phase extraction combined with fully automatic solid phase extraction-gas chromatography-mass spectrometry

作　　者：张念华[1] 王军淋[1] 冯靓[1] 应英[1] 赵永信[1] 堵雅芳 ZHANG Nian-hua;WANG Jun-lin;FENG Liang;YING Ying;ZHAO Yong-xin;DU Ya-fang(Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China;不详)

机构地区：[1]浙江省疾病预防控制中心,浙江杭州310051 [2]浙江中医药大学医学技术学院,浙江杭州310051

出　　处：《中国卫生检验杂志》2021年第1期24-27,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江省医药卫生科技计划项目(2018ZH005)。

摘　　要：目的建立全自动固相萃取-气相色谱-质谱法检测水中6种苯氧羧酸类除草剂的方法。方法取水样1 L,加抗坏血酸除余氯,经浓盐酸调节p H <1.0,加D3-2,4二氯苯氧乙酸(D3-2,4-D)内标后混匀,经全自动固相萃取仪上HLB固相萃取柱萃取,用二氯甲烷洗脱固相萃取柱上吸附的待测物,洗脱液氮吹至1 ml,用三甲基氢氧化硫溶液衍生,GC-MS分离检测。结果水样中的苯氧羧酸类除草剂的浓度在10μg/L~100μg/L线性良好,方法检出限为0.003μg/L,平均加标回收率为90.0%~103.1%,相对标准偏差(RSD)为3.15%~5.82%。结论该方法简便、准确,适用于水中6种苯氧羧酸类除草剂的检测。Objective To establish a method for the determination of six phenoxycarboxylic acid herbicides by automatic solid phase extraction-gas chromatography mass spectrometry( SPE-GC-MS) in drinking water. Methods After the removal of residual chlorine in the samples with ascorbic acid,the p H of the water samples( 1 L) were adjusted to less than 1. 0 with hydrochloric acid,then the analytes were extracted by HLB SPE cartridges,eluted with dichloromethane and concentrated to1. 0 ml under nitrogen flow. The analytes were derivatized with trimethyl sulfur hydroxide solution and finally detected by gas chromatography-mass spectrometry. Results Good linearity was obtained when the concentration of phenoxy carboxylic acid herbicides in water samples ranged from 10 μg/L to 100 μg/L,the detection limit was 0. 003 g/L,the average standard recovery was within 90. 0%-103. 1%,and the relative standard deviation( RSD) was within 3. 15%-5. 82%. Conclusion The method is quick and accurate and can be applied for the determination of six phenoxycarboxylic acid herbicides in drinking water.

关 键 词：生活饮用水 苯氧羧酸类除草剂 固相萃取法 气相色谱-质谱法 

分 类 号：O657.63[理学—分析化学]