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作 者:叶仕远[1] 叶雪梅[1] 王陈翔[1] 周子晔[1] 胡卢丰[1] 张秀华[1]
机构地区:[1]温州医学院附属第一医院药学部,浙江温州325000
出 处:《中国卫生检验杂志》2013年第1期46-48,共3页Chinese Journal of Health Laboratory Technology
摘 要:目的:建立高效、灵敏、快速的人血浆中百草枯的HPLC血药浓度测定方法。方法:以5-溴脲嘧啶为内标物,血浆经10%三氯乙酸甲醇去蛋白。采用XBridge-C18柱,流动相为乙腈-缓冲盐(V∶V,5∶95),缓冲盐为25.0 mmol/L磷酸二氢钠,含1.0 mmol/L十二烷基硫酸钠,pH 2.6,流速1.0 ml/min,检测波长258 nm,柱温35℃。结果:百草枯和内标的出峰时间分别为6.0 min和3.5 min,百草枯在0.05μg/ml~10μg/ml范围内线性关系良好(R2=0.9998)。低、中、高3种浓度的日内、日间精密度RSD均<6%,相对回收率100.623±5.443%,平均绝对回收率88.374±5.669%。结论:本方法操作简便易行,准确率高,可作为快速、准确测定人血浆中百草枯血药浓度的有效方法,为临床诊断提供依据。Objective:To establish a rapid and effective HPLC method for determination of paraquat in human plasma.Methods: The analytes in plasma were extracted by protein precipitation using 10% trichloroacetic acid and methanol(1∶ 1),with 5-bromine urea pyrimidine as internal standard,and separated at XBridge-C18.The mobile phase was acetonitrile-buffer solution(V∶ V,5∶ 95) that contained 25.0 mmol/L sodium dihydrogen phosphate and 1.0 mmol/L sodium dodecyl sulfate,pH was adjusted to 2.6,the flow rate was 1.0 ml/min,the UV detection wavelength was 258 nm,column temperature was 35℃.Results: The retention time of paraquat and internal standard was 6.0 min and 3.5 min.The calibration curves were linear in the range of 0.05 μg/ml~10 μg/ml(R2=0.9998).The intra and inter-day variations were less than 6%,relative recovery and absolute recovery were 100.623±5.443% and 88.374 ±5.669%.Conclusion: The established method is simple,sensitive and accurate for determining paraquat level in human plasma.
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