尿中氯苯代谢产物对氯苯酚测定的固相萃取-气相色谱法  

Determination of chlorobenzene metabolite-p-chlorophenol in urine by solid phase extraction-gas chromatography

作　　者：王鹏 曹艺耀[1] 任鸿 高向景[1] 徐秋凉 周振 Wang Peng;Cao Yiyao;Ren Hong;Gao Xiangjing;Xu Qiuliang;Zhou Zhen(Zhejiang Provincial Center for Disease Control and Prevention,Occupational Health and Radiation Protection Institute,Hangzhou 310051,China)

机构地区：[1]浙江省疾病预防控制中心职业健康与辐射防护所,杭州310051

出　　处：《中华劳动卫生职业病杂志》2022年第9期703-706,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：浙江省基础公益研究计划项目(LGC21H260001);浙江省卫生健康科技计划(2021KY613、2021KY616、2022KY132、2022KY130、2022RC120、2022ZH030)。

摘　　要：目的建立固相萃取-气相色谱法测定尿中氯苯代谢产物-对氯苯酚浓度的方法。方法于2021年5月,尿样中加入2 ml浓盐酸后在100℃下水解1.5 h,冷却过滤后经Oasis®MAX 6cc固相萃取小柱富集、净化。0.01 mol/L盐酸溶液淋洗,乙腈洗脱,洗脱液用乙腈定容至5 ml后气相色谱测定,标准曲线法定量。结果在1.61~80.30μg/ml浓度范围线性关系良好,线性回归方程为y=1.51602x-0.10234,相关系数为0.9997,方法的检出限为0.17μg/ml,定量下限为0.55μg/ml,方法加标回收率为89.3%~104.4%,日内测定相对标准偏差(RSD)为4.3%~6.7%,日间测定RSD为4.5%~6.7%。结论本方法优化了样品前处理,排除了杂质的干扰,测定灵敏、高效、准确,可用于尿中氯苯代谢产物-对氯苯酚的测定。Objective A method to determine chlorobenzene metabolite-p-chlorophenol in urine by solid phase extraction-gas chromatography was established.Methods In May 2021,the urine sample was hydrolyzed at 100℃for 1.5 h with 2 ml concentrated hydrochloric acid.After cooling and filtering,the sample was enriched and purified by Oasis®MAX 6cc SPE column.Drip washing with 0.01 mol/L hydrochloric acid solution and elution with acetonitrile,the eluent was volumized to 5 ml with acetonitrile and determined by gas chromatography,and quantify by standard curve method.Results Calibration curve of the method was linear within the range of 1.61-80.30μg/ml and showed good linearity with r=0.9997,the regression equation was y=1.51602x-0.10234.The determination limit was 0.17μg/ml,and the limit of quantitation was 0.55μg/ml.Recovery rates were between 89.3%-104.4%,the relative standard deviation(RSD)of intra-day measurements ranged from 4.3%to 6.7%,and the RSD of inter-day measurements ranged from 4.5%to 6.7%.Conclusion This method could optimize sample pretreatment,and eliminate the interference of impurities,which is sensitive,efficient and accurate for the determination of chlorobenzene metabolite-p-chlorophenol in urine.

关 键 词：固相萃取 色谱法 气相 尿液 对氯苯酚 氯苯 代谢产物 

分 类 号：R446.12[医药卫生—诊断学]