毛细管气相色谱法测定血浆、尿及指甲中的砷  

Determination of Arsenic in Plasma, Urine and Nail by Capillary Gas Chromatography

作　　者：秦燕[1] 庄慧娣[1] 吕勤 何平 

机构地区：[1]上海第二医科大学测试中心,上海200025 [2]上海二医爱尔药物研究和临床药理中心有限公司

出　　处：《上海第二医科大学学报》2003年第4期325-327,共3页Acta Universitatis Medicinalis Secondae Shanghai

摘　　要：目的建立毛细管气相色谱法测定血浆、尿及指甲中砷 (As)的方法。　方法血浆、尿及指甲处理后 ,As(Ⅲ )在酸性条件下与二巯基丙醇 (BAL)反应 ,经甲苯萃取 ,在气相色谱上直接进样。色谱柱为OV - 17弹性石英毛细管色谱柱 ,柱温 14 0℃～2 10℃ ,进样口温度 2 5 0℃ ,检测器温度 2 80℃ ,载气为高纯氮 ,流速为 2 .4ml/min ;63 Ni电子捕获检测器。　结果As的线性范围为 0 .0 2 ～10 μg/ml(r =0 .9996 ) ,最低检测浓度0 .0 0 35 μg/ml,低、中、高浓度加样回收率97.5 % ～99.7%之间。精密度考察As日内、日间相对标准差均小于 5 .1%。　结论本方法精密、准确 ,灵敏度高 。Objective A method for determination of arsenic in plasma, urine and nail by capillary gas chromatography has been established and validated. Methods As(Ⅲ) was reacted with dimercaptopropanol(BAL) under acidic conditions. As-BAL was extracted with toluene. Chromatography was performed on a OV-17 fused-silica capillary column with a 63 Ni electron capture detector. The column tempe rature was from 140℃ to 210℃, the injector temperature was 250℃ and the detector temperature was 280℃. The N 2 flow rate was 2.4ml/min. Results The standard curve was linear in the range 0.02～10μg/ml ( r =0.9996). The lowest detectable concentration was 0.0035 μg/ml. The additive recovery was between 97.5% ～99.7%. The within-day relative standard deviation(RSD) and between-day RSD were all less than 5.1%. Conclusion This method has good selectivity, sensitivity and reproducibility. It is suitable for clinical research and application.

关 键 词：砷 毛细管气相色谱法 血浆 尿 指甲 

分 类 号：O657.8[理学—分析化学]