| 曹银,梁俊,夏清荣,等.高效液相色谱法测定人血清中地西泮血药浓度及临床监测[J].安徽医药,2017,21(2):241-244. |
| 高效液相色谱法测定人血清中地西泮血药浓度及临床监测 |
| Concentration determination of diazepam in human serum by HPLC and clinical application |
| 投稿时间：2016-07-30 |
| DOI： |
| 中文关键词: 地西泮 氯氮平 高效液相色谱法 人血清 血药浓度 |
| 英文关键词: Diazepam Clozapine HPLC Human serum Plasma concentration |
| 基金项目: |
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| 摘要点击次数: 2441 |
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| 中文摘要: |
| 目的 建立人血清中地西泮浓度测定的高效液相色谱法(HPLC),并用该法测定临床病人静脉滴注地西泮后的血药浓度。方法 人血清样品采用正戊烷萃取进行分析。色谱柱:SB-C18色谱柱(150 mm×4.6 mm,5 μm),流动相为甲醇-水-四甲基乙二胺-冰醋酸(670∶330∶2.2∶1.76),柱温:40 ℃,流速:0.8 mL·min-1,检测波长:254 nm,进样量:20 μL。 以氯氮平作为内标物。结果 地西泮在10～1 200 μg·L-1浓度范围内,峰面积与其浓度呈良好的线性关系(r＝0.998 47),定量下限为10 μg·L-1。地西泮的高、中、低3种浓度相对平均回收率>95%,提取回收率均>70%,日内、日间的RSD均<15%(n=5)。地西泮稳定性考察RSD均<15%(n=5)。地西泮线性方程:Y=2 205.2X+1 876.1(r=0.998 47)。临床20例病人分别滴注地西泮20 mg,1 d 2次,前5 d早晨治疗前采血均检测出地西泮血药浓度。结论 该方法灵敏度高,操作简便、快速、准确,可用于人血清中地西泮血药浓度监测,并为临床病人个体化给药提供参考。 |
| 英文摘要: |
| Objective To establish a HPLC method for determination of diazepam concentration in human serum and determination of the plasma concentration in clinical patients after intramuscular injection of diazepam.Methods Human serum samples were extracted by 5 mL n-pentane and analyzed.Column:SB-C18 column (150 mm×4.6 mm,5 μm);Mobile phase:methanol- water- tetramethylethylenediamine- acetic acid (670∶330∶2.2∶1.76);The column temperature was 40 ℃;Flow rate:0.8 mL·min-1;and the detection wavelength was 254 nm;Injection volume was 20 μL.Clozapine was used as internal standard.Results The calibration curves were linear in the range of 10-1 200 μg·L-1 for diazepam(r＝0.998 47).The lower limit of quantification was 10 μg·L-1.The average recoveries of diazepam at high,middle and low concentration over 95%,the extraction recovery over 70%.The intra-day and inter-day RSD were less than 15% (n=5).The diazepam stability of RSD were less than 15% (n=5).The calibration curve of good linearity,r= 0.998 47.The regression equation of paroxetine was Y= 2 205.2X+1 876.1.After 20 patients were clinical intramuscular injection of diazepam 20 mg bid,before five days the morning treatment for determination of diazepam concentration in human serum.ConclusionsThe method is sensitive,simple,rapid,accurate and can be used for determination of diazepam concentration in human serum and can provide reference for clinical patient individualized. |
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