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HPLC法测定艾司唑仑血药浓度的方法验证

Method Validation of Plasma Concentration Determination of Estazolam by HPLC

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【作者】 侯大平张志国国玉芝雷力力黄展

【Author】 HOU Da-ping,ZHANG Zhi-guo,GUO Yu-zhi,LEI Li-li,HUANG Zhan(The First Affiliated Hospital of Jiamusi University,Jiamusi 154002,China)

【机构】 佳木斯大学附属第一医院

【摘要】 目的:建立测定艾司唑仑血药浓度的方法,以确定较好的检测条件。方法:采用高效液相色谱法,以依利特Hypersil ODS2 C18为色谱柱,甲醇-乙腈-水(28∶28∶54)为流动相,1.0 mL·min-1为流速,35℃为柱温,230 nm为检测波长,地西泮为内标,考察服用艾司唑仑片患者血浆、碱化血浆、血清浓度并对选定的标本及提取方法进行验证。结果:艾司唑仑血浆浓度明显高于碱化血浆及血清浓度,经成对双侧t检验,艾司唑仑血浆浓度与碱化血浆及血清浓度比较(P分别为0.011 30、0.018 17),有显著性差异。艾司唑仑血药浓度在0.049 4~1.289 6μg·mL-1范围内线性关系良好(r=0.991 8),定量下限为0.049 4μg·mL-1;平均日内、日间RSD均<10%,平均回收率为99.95%~100.79%。结论:采用患者血浆作为标本进行艾司唑仑血药浓度监测和药物中毒的定量分析可行,本方法简便、准确。

【Abstract】 OBJECTIVE:To establish the method for plasma concentration determination of estazolam,and to confirm optimal determination conditions.METHODS:HPLC method was adopted.The determination was performed on Elite Hypersil ODS2 C18 column with methanol-acetonitrile-water(28:28:54) as mobile phase at flow rate of 1.0 mL·min-1.The column temperature was set at 35 ℃ and detection wavelength was 230 nm.Diazepam was used as the internal standard.The concentrations of estazolam in plasma,alkalinized plasma and serum in patients receiving estazolam were determined.Selected samples and extraction method were verified.RESULTS:Plasma concentration of estazolam was significantly higher than those in alkalinized plasma and serum.In bilateral paired t test,the concentration of estazolam in plasma was significantly different from that in alkalinized plasma and serum(P=0.011 30 and P=0.018 17).The linear range of estazolam was 0.049 4~1.289 6 μg·mL-1(r=0.991 8).The minimum quantitation limit was 0.049 4 μg·mL-1.The average recovery rate was 99.95%~100.79%.The RSD of intra-day and inter-day were less than 10%.CONCLUSION:It is feasible to collect plasma sample of patients for plasma concentration monitoring of estazolam and quantitation analysis of drug poisoning.The method is simple,accurate.

  • 【分类号】R969.1
  • 【被引频次】5
  • 【下载频次】303
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