摘要
目的采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定云南省元谋县村民尿液中农药残留。方法尿液经Waters Oasis MCX柱固相萃取,用甲醇和5%的氨水甲醇溶液洗脱后离心浓缩,乙腈定容;以0.01%的甲酸乙腈溶液和0.01%的甲酸水溶液为流动相等梯度洗脱,经Cosmosil色谱柱(150 mm×4.6 mm)分离,采用电喷雾离子源正离子模式检测。结果方法的线性范围为0μg/ml^1.0μg/ml,相关系数(r)均>0.990;230份尿样中检测出多菌灵、异菌脲、百菌清、福美双、甲氰菊酯、高效氯氟氰菊酯、毒死蜱7种农药残留,其中150份尿液中检出有农药残留,检出阳性率为65.2%;异菌脲的检出率最高,为44.4%。结论该地居民尿液中农药残留检出率较高,是当地居民农药内暴露的直接证据,为评估农药职业暴露健康风险提供了依据。
Objective To determine the pesticide residues in urine from the rural residents in Yuanmou county,Yunnan by ultra performance liquid chromatography tandem mass spectrometry（ UHPLC-MS/MS）. Methods The urine samples were solid-phase extracted with Waters Oasis MCX,eluted with methanol and methanol-water containing 5% ammonia and quantified with acetonitrile. After centrifugation and concentration,the urine samples were separated on Cosmosil packed column（ 150 mm × 4. 6 mm） with acetonitrile-0. 01% formic acid and 0. 01% formic acid as mobile phase for constant gradient elution. Electrospray ionization source was applied and operated in positive ion mode. Results Within 0 μg/ml-1. 0 μg/ml,the correlation coefficient（ r） of the method were greater than 0. 990. Seven pesticide including carbendazim,iprodione,chlorothalonil,thiram,fenpropathrin,lambda-cyhalothrin and chlorpyrifos were detected in 230 urine samples,and 150 urine samples were detected with pesticide residues,and the positive rate was 65. 2%. The detection rate of lprodione was the highest as44. 4%. Conclusion The detection rate of pesticide residues in urine is high,which is the direct evidence of pesticide exposure in local residents,which provides a basis for assessing the health risk of pesticide occupational exposure.
作者
关秋艳
方菁
杨万群
孙晓
窦迎春
郝恩源
GUAN Qiu -yan＊ FANG Jing YANG Wan -qun SUN Xiao DOU Ying -chun HAO En -yuan(Institute for Health Sciences, Kunming Medical University, Kunmin, Yunnan 650500, Chin)
出处
《中国卫生检验杂志》
CAS
2016年第23期3350-3352,3356,共4页
Chinese Journal of Health Laboratory Technology
基金
加拿大国际发展研究中心资助的FBLI国际合作项目(106556-004)
关键词
农药
尿液
超高效液相色谱-串联质谱法
Pesticide residues
Urine
Ultra performance liquid chromatography tandem mass spectrometry
