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直接蛋白沉淀-超高效液相色谱法测定氟尿嘧啶血药浓度

袁文博, 丁永娟, 徐静静

袁文博, 丁永娟, 徐静静. 直接蛋白沉淀-超高效液相色谱法测定氟尿嘧啶血药浓度[J]. 中国药科大学学报, 2015, 46(1): 81-84. DOI: 10.11665/j.issn.1000-5048.20150111
引用本文: 袁文博, 丁永娟, 徐静静. 直接蛋白沉淀-超高效液相色谱法测定氟尿嘧啶血药浓度[J]. 中国药科大学学报, 2015, 46(1): 81-84. DOI: 10.11665/j.issn.1000-5048.20150111
YUAN Wenbo, DING Yongjuan, XU Jingjing. Determination of 5-fluorouracil in serum by direct protein precipitation-ultra performance liquid chromatography[J]. Journal of China Pharmaceutical University, 2015, 46(1): 81-84. DOI: 10.11665/j.issn.1000-5048.20150111
Citation: YUAN Wenbo, DING Yongjuan, XU Jingjing. Determination of 5-fluorouracil in serum by direct protein precipitation-ultra performance liquid chromatography[J]. Journal of China Pharmaceutical University, 2015, 46(1): 81-84. DOI: 10.11665/j.issn.1000-5048.20150111

直接蛋白沉淀-超高效液相色谱法测定氟尿嘧啶血药浓度

基金项目: 无锡市科技发展医疗卫生指导性计划资助项目(No.CSZON1311)

Determination of 5-fluorouracil in serum by direct protein precipitation-ultra performance liquid chromatography

  • 摘要: 建立直接蛋白沉淀-超高效液相色谱法测定血浆中微量氟尿嘧啶的方法。以6%高氯酸为沉淀剂,5-氯尿嘧啶为内标物,样品经涡旋振荡等处理后,高速离心获取上清液作为供试液。供试液测定采用Acquity HSS T3色谱柱,水-乙腈为流动相,流速为0.2 mL/min,进样量为5 μL,柱温为20 ℃。方法的专属性、准确度、精密度、线性等指标经验证后完全符合定量测定要求,与传统的测定方法相比,可显著缩短进样分析时间、降低试剂成本。本方法已经被成功用于临床病人的血药浓度检测,具有良好的临床应用前景。
    Abstract: A method based on direct protein precipitation-ultra performance liquid chromatography was established for the determination of trace 5-fluorouracil in serum. The samples were pretreated with 6% perchloric acid as the precipitant and 5-chlorouracil as the internal standard, and the supernatant separated after vortex mixing and high speed centrifugation was used as the test sample. The separation was carried out with an Acquity HSS T3 column and the mobile phase consisting of water and acetonitrile, and the flow rate was 0. 2 mL/min; the injection volume was 5 μL, and the column temperature was 20 °C. The key parameters of this method such as specificity, accuracy, precision and linearity, were validated. Compared with other methods, this method can complete the analysis with significantly reduced time and cost. The established method is useful for therapeutic drug monitoring of 5-fluorouracil plasma concentration and it has been successfully applied in clinical cases.
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  • 刊出日期:  2015-02-24

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