摘要
本文报道了一种反相高效液相色谱法 ,可同时测定氯氮平、去甲氯氮平、多塞平、去甲多塞平、阿米替林和去甲替林的血清浓度。本法选用IntersilODS -3柱为固定相 ,甲醇、乙腈和正丁胺 -冰醋酸缓冲液的混合液(5:35:60)为流动相 ,去甲米帕明为内标 ,紫外检测波长254nm。1ml待测血清加内标后 ,经0.5ml1mol·L -1NaOH碱化 ,加重蒸乙醚4ml提取 ,再用1ml0.2mol·L -1HCl反提取 ,最后经1ml2mol·L-1 NaOH碱化后用4ml重蒸乙醚提取 ,氮气吹干 ,流动相重组后进样分析。本法对各被测物的最低检测限在3~10ng之间 ,最低检测浓度在6~16μg·L-1 之间 ,提取回收率在65 %~81 %之间 ,批内和批间变异系数均小于10 % ,线性范围至少在25~800μg·L-1 之间。本法不受常用精神药物及其它药物的干扰 ,并已用于临床治疗药物监测工作和研究工作。
A reversed-phase HPLC method was reported for the simultaneous determination of clozapine, norclozapine, doxepin, nordoxepin, amitriptyline and nortriptyline in serum. An intersil ODS-3 column was used as the solid phase. The mobile phase was composed of methanol, acetonitrile and n-butylamine-acetic acid buffer (5:35:60). The separated drugs were detected at UV 254 nm. Desipramine was used as the internal standard. After adding the internal standard, 1 ml of patient serum was basified with 0.5 ml of 1mol·L-1 sodium hydroxide solution. 4 ml distilled diethyl ether was used to extract the drugs. Adding 1 ml of 0.2 mol·L-1 hydrochloric acid to the organic phase and extracted, the aqueous phase was re-basified with 1ml of 2 mol·L-1 sodium hydroxide solution and re-extracted with 4 ml distilled diethyl ether. This organic phase was evaporated to dryness by a stream of nitrogen. The residue was reconstituted with 50 μl mobile phase and injected into the HPLC system for analysis. The lowest detection limits of the drugs assayed are 3~10 ng. The level of determination was 6~16 μg·L-1 in serum. The extraction recoveries were 65%~81%. The interassay and intraassay variance was less than 10%. The standard curves were linear at list within the range of 25~800 μg·L-1 of all these drugs. This assay was not interfered by routine psychotropic drugs and other drugs. It has been used for the therapeutic drug monitoring of these drugs and research works.
出处
《中国临床药理学杂志》
CAS
CSCD
北大核心
1999年第5期369-373,共5页
The Chinese Journal of Clinical Pharmacology
关键词
氯氮平
三环类抗抑郁药
去甲基代谢物
血药浓度
clozapine
tricyclic antidepressants
therapeutic drug monitoring
high performance liquid chromatography
serum