分散固相萃取-超高效液相色谱-串联质谱法测定农产品中乙拌磷及其代谢物  

Determination of disulfoton and its metabolites in agricultural products by dispersive soild phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：孙强 李玉博[1] 温广月[1] 王伟民[1] 董茂锋[1] 唐红霞[1] SUN Qiang;LI Yubo;WEN Guangyue;WANG Weimin;DONG Maofeng;TANG Hongxia(Pesticide Safety Evaluation Research Center, Institute for Agro-Food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201106, China)

机构地区：[1]上海市农业科学院农药安全评价研究中心,上海市农业科学院农产品质量标准与检测技术研究所,上海201106

出　　处：《色谱》2022年第2期130-138,共9页Chinese Journal of Chromatography

基　　金：沪农科创字(2021)第3-2号.

摘　　要：基于超高效液相色谱-串联质谱(UHPLC-MS/MS)建立定量分析乙拌磷及其5个代谢物(乙拌磷砜、乙拌磷亚砜、内吸磷-S、内吸磷-S-砜、内吸磷-S-亚砜)的方法,应用该方法分析其在农产品(豌豆、芦笋、小麦、咖啡豆和花生)中的残留量。对样品前处理及色谱条件进行优化,样品经过乙腈涡旋提取(小麦、咖啡豆和花生先加水润湿),经盐析分层,取上清液经50 mg C_(18)、50 mg PSA和50 mg NH_(2)混合分散固相萃取净化后,经Thermo Syncronis C_(18)色谱柱(150 mm×2.1 mm,5μm)分离,柱温40℃,进样量2μL,以水和乙腈为流动相梯度洗脱后,采用ESI源,在正离子扫描和多反应监测(MRM)模式下检测,外标法定量。结果表明,乙拌磷及其代谢物在2.0~200.0μg/L范围内线性关系良好,相关系数(R^(2))≥0.9981。方法的检出限(LOD)为0.02~2.0μg/kg,并以最小添加水平5μg/kg为定量限(LOQ)。乙拌磷及其代谢物在豌豆、芦笋、小麦、咖啡豆和花生中5、100、1000μg/kg 3个添加水平下的平均回收率为75.0%~110.0%,相对标准偏差(RSD)为0.7%~14.9%,方法的准确度和精密度符合农药残留测定。应用建立的方法对市售的40份小麦样品和40份花生样品进行检测,均低于方法的检出限。该方法具有操作简单、快速、灵敏、准确的特点,适用于谷物、油料、蔬菜等多种农产品中乙拌磷及其代谢物的残留检测。Disulfoton,an organophosphorus pesticide,is used to control cotton,beet,potato,and other seedling period aphids,leaf moths,underground pests,etc.,with internal absorption,killing,gastric poisoning,and fumigation.Disulfoton is a highly toxic organophosphate pesticide,which can inhibit cholinesterase activity,resulting in neurophysiological disorders by inhalation,feeding,and transdermal absorption.Disulfoton is difficult to degrade in the environment,which leads to enrichment in organisms and interference with endocrine.This compound is harmful to the ecological environment and human health.To ensure the quality and safety of food,it is important to develop a detection method for disulfoton and its metabolites in agricultural products.A reliable method based on dispersive solid phase extraction(d-SPE)with ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was developed for the determination of disulfoton and its metabolites(disulfoton sulfone,disulfoton sulfoxide,demeton-S,demeton-S sulfone,and demeton-S sulfoxide)in agricultural products(pea,asparagus,wheat,coffee bean,and peanut).The optimal extraction method was as follows:5.0 g the samples were extracted with acetonitrile(wheat,coffee bean,and peanut presoaked in 5 mL water)in a 50 mL centrifuge tube,followed by 10 min vortex.Before 30 s vortex,4 g NaCl was added.After 5 min centrifugation,1.5 mL of the supernatant was cleaned up with 50 mg octadecylsilane bonded silica(C_(18)),50 mg primary secondary amine(PSA),and 50 mg aminopropyl(NH_(2))adsorbents.The analytes were separated on a Thermo Syncronis C18 column(150 mm×2.1 mm,5μm)with gradient elution using water and acetonitrile at a column temperature of 40℃.The injection volume was 2μL.Disulfoton and its metabolites were analyzed in multiple reaction monitoring(MRM)mode with positive electrospray ionization(ESI+)for the selective quantification.Qualitative and quantitative analyses were accorded to the retention times and characteristic ion pairs with one parent ion and tw

关 键 词：超高效液相色谱-串联质谱 分散固相萃取 乙拌磷 代谢物 农产品 

分 类 号：O658[理学—分析化学]