超声提取-多重净化-气质联用分析中华圆田螺中莠去津及其代谢物  

Determination of atrazine and its metabolites in Cipangopaludina chinensis by GC-MS with ultrasonic extractionand multiple purification

作　　者：孔祥吉[1,2] 田丰 张雪梅[3] 郭欣妍 吴文铸[1,2] 孔德洋[1,2] 

机构地区：[1]环境保护部南京环境科学研究所,南京210042 [2]国家环境保护农药环境评价与污染控制重点实验室,南京210042 [3]江苏省计量科学研究院,南京210007

出　　处：《分析试验室》2017年第11期1347-1350,共4页Chinese Journal of Analysis Laboratory

摘　　要：建立了中华圆田螺中莠去津(ATZ)及其主要代谢物脱乙基莠去津(DE-ATZ)、脱异丙基莠去津(DI-ATZ)和脱乙基-脱异丙基莠去津(DEDI-ATZ)的GC-MS分析方法。样品经乙腈匀浆、超声提取后,经由中性氧化铝,ZnSO_4,Na_2SO_4组成的层析柱脱脂、脱蛋白和脱水净化处理,使用HP-5毛细管柱在TIC模式下定性,SIM模式下外标法定量检测。测定结果表明,4种物质质量浓度在0.01~2 mg/L范围内线性良好,相关系数(r2)均≥0.999,方法检出限均为3μg/kg。加标回收率70%~109%,相对标准偏差(RSD)均低于9.6%(n=5)。方法用于测定城市景观湖内中华圆田螺中的ATZ及代谢物,表明ATZ和DI-ATZ均有检出。The method for the determination of atrazine and its main metabolites deethylatrazine （DE- ATZ ）, deisopropylatrazine （ DI-ATZ ）, and deethyldeisopropylatrazine （ DEDI-ATZ ） in Cipangopaludina chinensis using gas chromatography-mass spectrometry （GC-MS） was developed. The sample was first homogenated and ultrasonic extracted with acetonitrile, and then degreased, deproteinized and dehydrated by neutral alumina, anhydrous zinc sulfate, and anhydrous sodium sulfate, respectively. The object in the extraetwas detected qualitatively in TIC mode, and quantitatively with external standard method in SIM mode, both with HP-5 analyte column. It was indicated that the whole quantified curves of the 4 analytes had good linearity between 0.01 and 2 rag/L, and all the correlation coefficient （ r2 ） were above or equal to 0. 999 with all the determination limits of 3 μg/kg. All the recoveries of ATZ, DE-ATZ, DI-ATZ, and DEDI-ATZ were between 70% and 109% at 0. 01, 0. 1 and 1 mg/kg added concentrations with the relative standard deviations （RSDs） below 9. 6% （n = 5 ）in the additive recoveries test. After the Cipangopaludina chinensis in the inner lake was determinated by the method, it was indicated that ATZ and DI-ATZ were both detected, indicating that the study can supply an effective method for the determination of multi-pesticide residue in the Cipangopaludina chinensis.

关 键 词：GC-MS 莠去津及代谢物 中华圆田螺 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.53[轻工技术与工程—食品科学与工程]