尿中甲氧基乙酸测定的柱前衍生-液液微萃取-气相色谱法  

Determination of Methoxyacetic acid in urine by pre-column derivatization-liquid-liquid microextraction coupled with gas chromatography

作　　者：顾缨缨 梅勇[1,3] 苏婉婷 韩军[2] Gu Yingying;Mei Yong;Su Wanting;Han Jun(School of Public Health,Wuhan University of Science and Technology,Wuhan 430065,China;College of Resource and Environmental Engineering of Science and Technology,Wuhan 430065,China;Hubei Province Key Laboratory of Occupational Hazard Identification and Control,Wuhan University of Science and Technology,Wuhan 430065,China)

机构地区：[1]武汉科技大学医学院公共卫生学院,430065 [2]武汉科技大学资源与环境工程学院,430065 [3]武汉科技大学职业危害识别与控制湖北省重点实验室,430065

出　　处：《中华劳动卫生职业病杂志》2021年第8期602-605,共4页Chinese Journal of Industrial Hygiene and Occupational Diseases

摘　　要：目的建立乙二醇单甲醚的代谢产物尿中甲氧基乙酸的柱前衍生-液液微萃取-气相色谱测定法。方法向尿样中加入磷酸盐缓冲液、叔丁氧基乙酸(内标物)、五氟苄基溴(衍生剂),随后置于90℃水浴锅中衍生40 min,冷却后过滤,二氯甲烷萃取,振荡离心后吸取下层有机相注入气相色谱仪,DB-5毛细管色谱柱分离,ECD检测器检测。结果尿中甲氧基乙酸浓度在0.6~60.0 mg/L时线性关系良好,相关系数>0.999,平均回收率为76.6%~110.7%,日间精密度为8.00%~8.82%,检出限为0.13 mg/L。结论该方法灵敏度高,有机试剂用量少,适用于职业接触乙二醇单甲醚人群尿中甲氧基乙酸的检测。Objective To establish a method for determining methoxyacetic acid in urine by pre-column derivatization-liquid-liquid microextraction coupled with gas chromatography(GC).Methods Phosphate buffer solution,tert-butoxyacetic acid(internal standard)and pentafluorobenzyl bromide(derivative)were added to the urine sample.After derived in a water bath at 90℃for 40 min,the mixture was cooled and filtered,then the dichloromethane was used as an extractant.After being shaken and centrifuged,the lower organic phase was sucked and injected into a gas chromatograph,separated by a DB-5 capillary column,and detected by an ECD detector.Results The linear range of the method was 0.6~60.0 mg/L with the correlation coefficients(r)above 0.999.The average recovery was76.6%~110.7%,the inter-day precision was 8.00%~8.82%,and the detection limit was 0.13 mg/L.Conclusion The method was founded to be high sensitivity,low organic reagent usage and green.So it is suitable for the detection of methoxyacetic acid in urine of occupational exposure to ethylene glycol monomethyl ether.

关 键 词：气相色谱 甲氧基乙酸 液液萃取 柱前衍生-液液微萃取 尿 

分 类 号：R446.12[医药卫生—诊断学]