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一种用于尿液中阿片类药物分离与鉴定的固相萃取技术。

A solid phase extraction technique for the isolation and identification of opiates in urine.

作者信息

Huang W, Andollo W, Hearn W L

机构信息

Dade County Medical Examiner Department, Miami, Florida 33136-1133.

出版信息

J Anal Toxicol. 1992 Sep-Oct;16(5):307-10. doi: 10.1093/jat/16.5.307.

Abstract

A quantitative method was developed for the simultaneous analysis of morphine, codeine, hydromorphone, hydrocodone, and oxycodone in urine by gas chromatography/mass spectrometry. Samples were hydrolyzed with beta-glucuronidase and then extracted by solid phase extraction on Bond Elute Certify cartridges at pH 6.8. Nalorphine was used as the internal standard. The opiates were analyzed by full-scan electron impact GC/MS after derivatization with acetic anhydride-pyridine. The standard curves for all five drugs were linear between 50 and 1000 ng/mL, with correlation coefficients exceeding 0.99. Coefficients of variation were less than 7%. The method was applied to the analysis of postmortem urines positive by EMIT opiate assay, and the effect of the hydrolysis procedure on recovery of each drug was measured. The results indicate that the hydrolysis procedure is effective in increasing the recovery of all five drugs from urine. The described method enables the laboratory to identify the five opiates most commonly encountered in forensic and clinical laboratories. Its sensitivity for all five drugs is well below GC/MS cutoffs for codeine and morphine employed in NIDA laboratories, and it provides for conclusive full-scan drug identification.

摘要

建立了一种气相色谱/质谱法同时分析尿液中吗啡、可待因、氢吗啡酮、氢可酮和羟考酮的定量方法。样品用β-葡萄糖醛酸酶水解,然后在pH 6.8条件下于Bond Elute Certify柱上进行固相萃取。烯丙吗啡用作内标。用乙酸酐-吡啶衍生化后,通过全扫描电子轰击气相色谱/质谱法分析阿片类药物。所有五种药物的标准曲线在50至1000 ng/mL之间呈线性,相关系数超过0.99。变异系数小于7%。该方法应用于经EMIT阿片类药物检测呈阳性的死后尿液分析,并测定了水解程序对每种药物回收率的影响。结果表明,水解程序可有效提高尿液中所有五种药物的回收率。所述方法使实验室能够鉴定法医和临床实验室中最常遇到的五种阿片类药物。其对所有五种药物的灵敏度远低于美国国家药物滥用研究所(NIDA)实验室用于可待因和吗啡的气相色谱/质谱法临界值,并且能够进行确凿的全扫描药物鉴定。

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