尿中正丁醇测定的顶空固相微萃取-气相色谱法

来源 :中华劳动卫生职业病杂志 | 被引量 : 0次 | 上传用户:ariesping
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目的:建立顶空固相微萃取-气相色谱法测定尿中正丁醇的含量。方法:于2019年10月,用聚二甲基硅氧烷/二乙烯苯(PDMS/DVB)固相微萃取头萃取尿中正丁醇,优化盐析量、萃取温度、萃取时间和解吸时间,用HP-5毛细管柱(30 m×0.32 mm×0.25 μm)分离,氢火焰离子化检测器(FID)检测,外标法定量。结果:尿中正丁醇在0.04~3.00 mg/L浓度线性关系良好,相关系数为0.999,方法的检出限为0.04 mg/L,回收率为77.4%~102.8%,批内精密度为3.67%~8.11%,批间精密度为4.94%~6.90%。结论:正丁醇测定方法操作简便,富集效率高,灵敏度高,适用于职业接触人群尿样中正丁醇含量的测定。“,”Objective:To establish a headspace solid phase microextraction-gas chromatography method for determination of n-Butyl alcohol in urine.Methods:In October 2019, the n-butyl alcohol in urine was extracted with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) solid-phase microextraction head. The conditions of salt amount, extraction temperature, extraction time and desorption time were optimized. The separation was performed on HP-5 (30 m×0.32 mm×0.25 μm) capillary column and detected with flame ionization detector. The quantification was based on the external standard curve.Results:The linear relationship of n-butyl alcohol in urine was good in the range of 0.04-3.00 mg/L, the correlation coefficient was 0.999, the detection limit of the method was 0.04 mg/L, the recovery was 77.4%-102.8%, the intra-run precision was 3.67%-8.11%, and the inter-assay precision was 4.94%-6.90%.Conclusion:The method has simple operation, high concentration efficiency and high sensitivity, and it is suitable for the determination of n-butyl alcohol in urine of occupational exposure to n-butyl alcohol.
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