Nakahara Y, Takahashi K, Sakamoto T, Tanaka A, Hill V A, Baumgartner W A
National Institute of Health Sciences, Tokyo, Japan.
J Anal Toxicol. 1997 Sep;21(5):356-62. doi: 10.1093/jat/21.5.356.
The paper reports the simultaneous detection hair of phencyclidine (PCP) and its two major metabolites, 1-(1-phenylcyclohexyl)-4-hydroxypiperidine (PCHP) and trans-1-(1-phenyl-4-hydroxycyclohexyl)-4'-hydroxypiperidine (t-PCPdiol) in human hair. The detection of these metabolites provides definitive evidence that a positive hair analysis result is due to active PCP use and not due to external contamination of the hair specimen. Hair (5 mg) from known PCP users was washed three times with 0.1% sodium dodecyl sulfate for 1 min before analysis. Three extraction methods were compared: methanol-5N HCl (20:1) (Method A), 10% HCl (Method B), and 2N sodium hydroxide digestion (Method C). PCP-d5 and PCHP-d5 were used as internal standards. Extracts were purified by Bond Elut Certify solid-phase extraction procedures. Samples were derivatized with N,O-bis-trimethylsilyl acetamide and analyzed by gas chromatography-mass spectrometry. Compared with Method A, the extraction efficiencies of Methods B and C for PCP were 83-89%; however, the extraction efficiencies of Methods B and C for the two metabolites were only half or less than that of Method A. Method A was therefore selected for the analysis of clinical hair specimens from eight PCP users. The coefficients of variation of this method (n = 5) for PCP at 4 ng/mg and for PCHP and t-PCPdiol at 0.2 ng/mg were 2.13, 6.09, and 9.38%, respectively. In the eight hair specimens, PCP values ranged between 0.33 and 14 ng/mg. PCHP between 0.02 and 0.12 ng/mg, and trans-PCPdiol between 0.09 and 0.45 ng/mg. It was found that t-PCPdiol was the major metabolite in the PCP users' hair specimens, although t-PCPdiol was a minor metabolite in the hair specimens of rats intoxicated with PCP.
该论文报道了在人发中同时检测苯环己哌啶（PCP）及其两种主要代谢物，即1-(1-苯基环己基)-4-羟基哌啶（PCHP）和反式-1-(1-苯基-4-羟基环己基)-4'-羟基哌啶（t-PCP二醇）。这些代谢物的检测提供了确凿证据，证明头发分析结果呈阳性是由于主动使用PCP，而非头发样本受到外部污染。来自已知PCP使用者的头发（5毫克）在分析前用0.1%十二烷基硫酸钠洗涤三次，每次1分钟。比较了三种提取方法：甲醇-5N盐酸（20:1）（方法A）、10%盐酸（方法B）和2N氢氧化钠消化法（方法C）。PCP-d5和PCHP-d5用作内标。提取物通过Bond Elut Certify固相萃取程序进行纯化。样品用N,O-双三甲基硅基乙酰胺衍生化，然后通过气相色谱-质谱联用仪进行分析。与方法A相比，方法B和C对PCP的提取效率为83 - 89%；然而，方法B和C对两种代谢物的提取效率仅为方法A的一半或更低。因此，选择方法A对8名PCP使用者的临床头发样本进行分析。该方法（n = 5）对4 ng/mg的PCP、0.2 ng/mg的PCHP和t-PCP二醇的变异系数分别为2.13%、6.09%和9.38%。在这8份头发样本中，PCP值在0.33至14 ng/mg之间，PCHP在0.02至0.12 ng/mg之间，反式PCP二醇在0.09至0.45 ng/mg之间。研究发现，t-PCP二醇是PCP使用者头发样本中的主要代谢物，尽管t-PCP二醇在PCP中毒大鼠的头发样本中是次要代谢物。
