环境大气颗粒物中草甘膦的加速溶剂萃取-离子色谱测定法  

Determination of glyphosate in atmospheric particulates by accelerated solvent extraction-ion chromatography

作　　者：何漪[1,2] 朱莎 刘月月 魏滨[1,2] 常通 王韬[1,2] HE Yi;ZHU Sha;LIU Yue-yue;WEI Bin;CHANG Tong;WANG Tao(Sanitary Inspection Department,Zibo Center for Disease Control and Prevention,Zibo Shandong,255026,China;Zibo Key Laboratory of Environmental Organic Pollution and Human Health Monitoring and Analysis,Zibo Shandong,255026,China)

机构地区：[1]淄博市疾病预防控制中心卫生检验科,山东淄博255026 [2]淄博市环境有机污染与人群健康监测分析重点实验室,山东淄博255026

出　　处：《职业与健康》2022年第24期3352-3355,共4页Occupation and Health

基　　金：山东省医药卫生科技发展计划项目(202112010542)。

摘　　要：目的 建立环境大气颗粒物中草甘膦的加速溶剂萃取-离子色谱测定方法。方法 取适量采样滤膜加纯水为萃取剂,压力为10 MPa,循环次数为2次,萃取温度选择50℃,快速溶剂萃取仪对滤膜样品进行萃取,萃取液进离子色谱仪检测,100μL进样量,35 mmol/L的氢氧化钾在线淋洗,再生抑制-电导检测器-离子色谱法进行测定,外标法定量。结果 所建立的检测方法对草甘膦在质量浓度为0.20~5.00 mg/L范围内与峰面积线性关系良好,相关系数≥0.999,方法检出限为0.033 mg/L,定量限为0.10 mg/L,相对标准偏差(RSD)为2.59%~6.02%,平均加标回收率为95.92%~106.40%。以采集空气样品体积120 000 L计算,该检测方法对环境大气中草甘膦的检测范围为0.002~0.050μg/m3,最低检出浓度为0.001μg/m3。结论 该方法灵敏度高、精密度好、准确度高、检出限低,适用于环境大气颗粒物中草甘膦的测定。Objective To establish a method for determination of glyphosate in atmospheric particulates by accelerated solvent extraction-ion chromatography. Methods The glyphosate on quartz fiber membrane was extracted by pure water through an accelerated solvent extractor. The extraction pressure was 10 MPa,the extraction temperature was 50 ℃ and the extraction process was repeated twice. The sample was determined by ion chromatograph with 100 μL sample load and 35 mmol/L KOH solution online leaching,the regeneration inhibition-conductance detector-ion chromatography was used for the determination,and external standard method for quantification. Results A good linear relation between the peak area and the concentration of glyphosate ranged from 0.20 to 5.00 mg/L was obtained with the established method,with the correlation coefficient ≥0.999. The detection limit was 0.033 mg/L and the limit of quantitation was 0.10 mg/L. The relative standard deviation(RSD) was 2.59%-6.02%,and the average recovery rate was 95.92%-106.40%. The detection range of glyphosate in atmospheric particulates was 0.002-0.050 μg/m~3 and the minimum detectable concentration was 0.001 μg/m~3(assuming that the sampling volume was 120 000 L).Conclusion This method has high sensitivity,precision,accuracy and low detection limit,it is suitable for the determination of glyphosate in atmospheric particulates.

关 键 词：加速溶剂萃取 大气颗粒物 草甘膦 离子色谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]