摘要
目的建立可同时测定人血清中利培酮、9-羟利培酮、氯氮平、去甲氯氮平和瑞波西汀5种药物浓度的高效液相色谱-紫外检测法,并将该方法用于临床急性精神药物中毒患者的血液样本分析。方法以乙醚为溶剂进行一步液液萃取,待测物与内标帕罗西汀在Inertsil ODS-3柱,乙腈∶甲醇∶正丁胺∶冰醋酸∶去离子水(20∶2.87∶1.07∶1∶34.29)条件下可以基线分离。线性范围100～1 600 ng/mL,最低检测限25μg/L(S/N=10)。结果本方法批内精密度为3.1%～15.6%,批间精密度为5.7%～18.4%;批内准确度为0.1%～8.7%,批间准确度为0.3%～13.3%。常见精神科药物不干扰待测药物和内标。结论本方法简单、特异性好,可应用于急诊患者药物中毒检测。
Objective A high performance liquid chromatography（HPLC） method with ultraviolet（UV） detection（230 nm） was developed and validated for the quantification of 5 drugs, Risperidone, clozapine, reboxetine, 9-hydroxy Risperidone and norclozapine, in human serum. Methods Following a one-step liquid-liquid extraction with diethyl ether, the analyte and internal standard（paroxetine） were separated using an isocratic mobile phase consisted of acetonitrile ：methanol ：butylamine ：acetic acid ：deionized water = 20：2.9：1.1： 1：34.3 on a reverse phase Inertsil C1s-3 column. Five drugs and IS were separated well under the chromatographic condition. The calibration curve was verified over the range of 100 - 1 600 μg,/L and limit of detection（LOD） was 25 μg/L（ S/N = 10）. Results The imprecision of within and between batches were 3.1% - 15.6% and 5.7% -18.4%, respectively. The accuracy of within and between batches were 0. 1% - 8.7% and 0.3% - 13.3%. Commonly used psychotropic drugs did not interfere with the drugs and internal standard. Conclusion This method was found to be rapid, simple, accurate, sensitive and more suitable for rapid qualitative and quantitative determination of drugs in the serum of overdosed patients.
出处
《首都医科大学学报》
CAS
2013年第2期270-274,共5页
Journal of Capital Medical University
基金
北京市委组织部优秀人才培养专项基金(2004)
首都医学科研发展基金(2009-3135)~~
关键词
过量中毒
液液萃取
高效液相色谱
overdose
liquid-liquid extraction
high performance liquid chromatography
