尿中环己醇测定的顶空-固相微萃取气相色谱法
Determination of cyclohexanol in urine by headspac e solid-phase microextr action coupled with gas chromatography
摘要目的 建立环己酮的代谢产物尿中环己醇的顶空-固相微萃取气相色谱测定方法.方法 尿样经β-葡萄糖苷酸酶水解后,加入2.0 g氯化钠,50℃水浴20 min,用碳烯/聚二甲基硅氧烷(CAR/PDMS)固相微萃取头吸附,将萃取头插入气相色谱测定,DB-5毛细管色谱柱分离,氢火焰离子化检测器检测.结果 尿中环己醇在0.10~5.00 mg/L浓度线性关系良好,r=0.999,平均回收率为84.5%~96.3%,日间精密度为3.81%~6.00%,检出限为0.03 mg/L.结论 该方法检出限低,操作简便,准确度高,无需有机溶剂,适用于职业接触环己酮人群尿中环己醇的检测.
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abstractsObjective To establish a method for determining cyclohexanol in urine by headspace solid-phase microextraction (HS/SPME) coupled with gas chromatography (GC). Methods After the urine sample was hydrolyzed by β-glucuronidase, 2.0 g of NaCl was added, then the analyte in urine was adsorbed by a CAR/PDMS solid phase micro-extraction head in a water bath at 50℃for 20 min. And the extraction head was inserted into the gas chromatograph gasification chamber to desorb, the analyte was detected after separated by the capillary through the flame ionization detector. Results The linear range of the method was 0.1-5.0 mg/L with the correlation coefficients(r) 0.999. The average recovery was 84.5%-96.3%, the inter-day precision was 3.81%-6.00%, and the detection limit was 0.03 mg/L. Conclusion The method is founded to be low detection limit, simple operation and no need of organic solvent. So it is suitable for the detection of cyclohexanol in urine of occupational exposure to cyclohexanone.
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