超高效液相色谱法测定血浆中倍硫磷及其主要代谢产物  

Determination of fenthion and its main metabolites in plasma by ultra-performance liquid chromatography

作　　者：谢玉璇 王子浩 李添娣 刘奋 郭翔 XIE Yuxuan;WANG Zihao;LI Tiandi;LIU Fen;GUO Xiang(Shenzhen Prevention and Treatment Center for Occupational Disease,Shenzhen,Guangdong 518020,China;School of Public Health,Jilin University,Changchun,Jilin 130021,China)

机构地区：[1]深圳市职业病防治院,广东深圳518020 [2]吉林大学公共卫生学院,吉林长春130021

出　　处：《职业卫生与应急救援》2024年第5期660-665,共6页Occupational Health and Emergency Rescue

基　　金：深圳市科技计划项目(JCYJ20220531091213031);深圳市职业病防治院科研培育计划项目(SZF-PY-2023-003);中华预防医学会中毒控制科研项目(CPMAZD2024006)。

摘　　要：目的建立血浆中倍硫磷及其5种代谢物(倍硫磷氧化物、倍硫磷砜、倍硫磷亚砜、倍硫磷氧砜和倍硫磷氧亚砜)的超高效液相色谱(UPLC)测定方法。方法取0.50 mL待测血浆经乙酸乙酯+乙腈混合溶液(体积比1∶1)萃取,氮气吹干,甲醇定容,采用ACQUITY UPLC BEH C18柱分离,以甲醇和甲酸水溶液为流动相梯度洗脱,二极管阵列检测器检测,以保留时间和吸收光谱定性,以峰面积外标法定量。结果倍硫磷及其5种代谢物在各自线性范围内相关性良好,相关系数为0.9998~0.9999;检出限0.1~0.2 mg/L,定量限0.3~0.6 mg/L,加标回收率为87.18%~111.02%。批内精密度为0.52%~9.86%,批间精密度为1.07%~7.19%。除倍硫磷氧砜外,样品可在-40℃保存7 d。结论本方法准确可靠,简便实用,可用于测定血浆中倍硫磷及其5种代谢物。Objective To establish a method for the determination of fenthion and its five metabolites(fenthion oxide,fenthion sulfone,fenthion sulfoxide,fenthion oxy-sulfone,and fenthion oxy-sulfoxide)in plasma using ultra-performance liquid chromatography(UPLC).Methods A volume of 0.50 mL plasma sample was extracted with a mixture of ethyl acetate and acetonitrile(1:1,v/v),evaporated to dryness under nitrogen,and reconstituted with methanol.Separation was performed on an ACQUITY UPLC BEH C18 column using a gradient elution with methanol and formic acid aqueous solution as the mobile phase.Detection was carried out with a diode array detector,with qualitative analysis based on retention time and absorption spectra and quantitative analysis using an external standard method based on peak area.Results Fenthion and its five metabolites showed good linearity within their respective ranges,with correlation coefficients of 0.9998 to 0.9999.The limits of detection were 0.1 to 0.2 mg/L,and the limits of quantification were 0.3 to 0.6 mg/L.The spiked recovery rates ranged from 87.18%to 111.02%.Intra-batch precision ranged from 0.52%to 9.86%,and inter-batch precision ranged from 1.07%to 7.19%.Except for fenthion oxy-sulfone,the plasma samples could be stored at-40°C for 7 days.Conclusions This method is accurate,reliable,simple,and practical for the determination of fenthion and its five metabolites in plasma.

关 键 词：倍硫磷 代谢产物 超高效液相色谱法 血浆 

分 类 号：R134.4[医药卫生—劳动卫生]