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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。
In this paper, an RP-HPLC method was developed for the simultaneous determination of serum concentrations of clozapine, norczapine, doxepin, norvalosin, amitriptyline and nortriptyline. In this method, IntersilODS-3 column was used as stationary phase. The mobile phase consisted of methanol, acetonitrile and n-butylamine-glacial acetic acid buffer (5:35:60). 1ml serum to be tested plus internal standard, basified by 0.5ml1mol·L -1NaOH, add steamed 4ml extraction, and then 1ml0.2mol·L -1 HCl anti-extraction, and finally alkalinized with 1ml2mol · L-1 NaOH with 4ml Re-steamed ether extract, dry nitrogen, the mobile phase re-injection analysis. The minimum detectable limit for each analyte in this method is between 3 and 10 ng, the lowest detectable concentration is between 6 and 16 μg · L-1, and the extraction recovery is between 65% and 81% Coefficients were less than 10%, the linear range of at least between 25 ~ 800μg · L-1. This law is not disturbed by commonly used psychotropic drugs and other drugs, and has been used for clinical treatment of drug monitoring and research work.