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通过离子阱质谱法定量测定有色和无色毛发中的苯环利定。

Quantitative determination of phencyclidine in pigmented and nonpigmented hair by ion-trap mass spectrometry.

作者信息

Slawson M H, Wilkins D G, Foltz R L, Rollins D E

机构信息

Department of Pharmacology and Toxicology, University of Utah, Salt Lake City 84112, USA.

出版信息

J Anal Toxicol. 1996 Oct;20(6):350-4. doi: 10.1093/jat/20.6.350.

DOI:10.1093/jat/20.6.350
PMID:8889669
Abstract

A sensitive and specific method has been developed for the quantitative analysis of phencyclidine (PCP) in pigmented and nonpigmented rat hair. After the addition of PCP-d5 as the internal standard, hair samples (10 mg) were digested overnight in 1N NaOH at 30 degrees C. Digested solutions were then extracted using a solid-phase procedure with Bond Elut CertifyTM extraction columns. Reconstituted extracts were analyzed on a Finnigan ion trap (MagnumTM) mass spectrometer in the electron ionization mode using helium as the carrier gas, and a DB-5 MS (30 m x 0.25-mm i.d.; 25-microns film thickness) capillary column. The assay is linear from 0.1 to 50 ng/mg with a correlation coefficient of > 0.99 and is capable of detecting 25 pg of PCP on column. The accuracy of this assay was estimated using fortified hair standards at PCP concentrations of 0.5 and 10 ng/mg. Intra-assay coefficients of variation were determined to be less than 6% at 0.5, 2, and 10 ng/mg. Interassay coefficients of variation were determined to be less than 15% at 0.5, 2, and 10 ng/mg. The method has been used to evaluate PCP incorporation into Long-Evans rat hair but could also be used to evaluate the incorporation of PCP into human hair. Male rats were shaved prior to dosing such that both pigmented and nonpigmented hair was collected. Animals were administered 12 mg/kg PCP by intraperitoneal injection daily for five days. Fourteen days after the first dose, pigmented and nonpigmented hair were collected and analyzed for PCP. The mean plus or minus the standard error of the mean (n = 5) concentrations of PCP in pigmented and nonpigmented hair were 14.33 +/- 1.43 ng/mg of hair and 0.47 +/- 0.04 ng/mg of hair, respectively. This method is also being used to evaluate PCP as a model xenobiotic for studies of the incorporation of xenobiotics into hair.

摘要

已开发出一种灵敏且特异的方法,用于定量分析有色和无色大鼠毛发中的苯环利定(PCP)。加入PCP-d5作为内标后,将毛发样品(10毫克)在30℃下于1N氢氧化钠中消化过夜。然后使用Bond Elut CertifyTM萃取柱通过固相萃取程序对消化后的溶液进行萃取。将重构后的萃取物在配备氦气作为载气的Finnigan离子阱(MagnumTM)质谱仪上,采用电子电离模式,并使用DB-5 MS(30米×0.25毫米内径;25微米膜厚)毛细管柱进行分析。该测定法在0.1至50纳克/毫克范围内呈线性,相关系数大于0.99,且能够在柱上检测到25皮克的PCP。使用PCP浓度为0.5和10纳克/毫克的加标毛发标准品来评估该测定法的准确性。在0.5、2和10纳克/毫克时,批内变异系数测定为小于6%。在0.5、2和10纳克/毫克时,批间变异系数测定为小于15%。该方法已用于评估PCP在Long-Evans大鼠毛发中的掺入情况,但也可用于评估PCP在人发中的掺入情况。在给药前将雄性大鼠剃毛,以便收集有色和无色毛发。动物每天通过腹腔注射给予12毫克/千克的PCP,持续五天。首次给药后十四天,收集有色和无色毛发并分析其中的PCP。有色和无色毛发中PCP的平均浓度(±平均标准误差,n = 5)分别为14.33±1.43纳克/毫克毛发和0.47±0.04纳克/毫克毛发。该方法也正被用于评估PCP作为一种模型外源性物质,用于研究外源性物质在毛发中的掺入情况。

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