Quantification of phencyclidine in body fluids by gas chromatography chemical ionization mass spectrometry and identification of two metabolites
Quantification of phencyclidine in body fluids by gas chromatography chemical ionization mass spectrometry and identification of two metabolites
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采用气相色谱化学电离质谱法定量体液中的苯环己哌啶并鉴定两种代谢物
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发表时间：
1975
期刊：
影响因子：
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通讯作者：
I. Sunshine
中科院分区：
文献类型：
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作者：
D. C. Lin;A. Fentiman;R. Foltz;Robert D. Forney;I. Sunshine
建立了一种用选择离子记录的气相色谱化学电离质谱法定量测定体液中苯环利定[1-（1-苯基环己基）哌啶]的方法。合成了五氘代苯环利定并用作内标。在开发该方法时，发现苯环利定在升高的温度下热裂解为1-苯基环己烯。该方法的灵敏度和特异性允许测定在1 ml体液中的1 ng苯环利定。从五个人的血液样本中，谁摄入了未知数量的苯环利定的药物浓度，发现范围从50纳克/毫升至2.7微克/毫升。对一只12.5 kg的狗静脉注射1 mg盐酸苯环利定后，药物的血药浓度峰值为17.6 ng/ml，半衰期约为1小时。酶解后，在人和犬尿液中检测到苯环利定的两种代谢产物。通过代谢产物及其三甲基硅基衍生物的电子轰击和化学电离质谱分析，初步鉴定代谢产物为4-苯基-4-哌啶基环己醇和1-（1-苯基环己基）-4-羟基-哌啶。通过代谢产物的合成实现结构确认。在恒河猴尿液中发现第三种代谢物，初步鉴定为1-（1-苯基-4-羟基环己基）-4-羟基哌啶。
A method has been developed for quantification of phencyclidine [1-(1-phenylcyclohexyl)piperidine] in body fluids using gas chromatography chemical ionization mass spectrometry with selected ion recording. Pentadeuterated phencyclidine was synthesized and used as the internal standard. In developing the method it was discovered that phencyclidine thermally fragments to 1-phenylcyclohexene at elevated temperatures. The sensitivity and specificity of the method permits determination of 1 ng of phencyclidine in 1 ml of body fluid. The concentrations of the drug in blood samples from five individuals, who ingested unknown quantities of phencyclidine, were found to range from 50 ng/ml to 2.7 μg/ml. Following intravenous administration of 1 mg of phencyclidine hydrochloride to a 12.5 kg dog, the blood concentration of the drug peaked at 17.6 ng/ml and exhibited a half-life of approximately one hour. Two metabolities of phencyclidine were detected in human and dog urine after enzymatic hydrolysis. The metabolities were tentatively identified as 4-phenyl-4-piperidinocyclohexanol and 1-(1-phenylcyclohexyl)-4-hydroxy-piperidine by electron impact and chemical ionization mass spectral analysis of the metabolites and their trimethylsilyl derivatives. Structural confirmation was achieved by synthesis of the metabolities. A third metabolite was found in urine from rhesus monkeys and was tentatively identified as 1-(1-phenyl-4-hydroxycyclohexyl)-4-hydroxypiperidine.