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一种检测和定量尿液中胍法辛的 HPLC-MS 方法。

A HPLC-MS method to detect and quantify guanfacine in urine.

机构信息

Department of Forensic Science, Virginia Commonwealth University, Richmond, VA, USA.

出版信息

Clin Chem Lab Med. 2011 Nov 24;50(3):535-7. doi: 10.1515/CCLM.2011.803.

DOI:10.1515/CCLM.2011.803
PMID:22112053
Abstract

BACKGROUND

Guanfacine, an α2-adrenergic α2A)agonist long indicated to treat hypertension, is now being used to treat attention deficit-hyperactivity disorder (ADHD) in adolescents. This new therapeutic use may require urine testing to document compliance or abuse. A simple rapid high pressure liquid chromatography-mass spectrometry (HPLC-MS) method to detect and quantify guanfacine in urine following therapeutic administration is presented.

METHODS

Guanfacine and protriptyline internal standard were extracted from alkalinized urine with ethyl acetate. The organic layer was evaporated, reconstituted with mobile phase and analyzed on a YMC Basic S-5 micron, 2.0 × 150 mm HPLC column connected to an MS detector operated in positive electrospray ionization mode with selected ion resonance. Elution times were <5 min.

RESULTS

The analytical measurement range for guanfacine was 20-2000 ng/mL. The limit of detection and quantitation were 5 ng/mL and 20 ng/mL, respectively. Precision as %CV was <15% at 40, 100 and 500 ng/mL (n=6). Percentage recovery using the same concentrations was >89%. Interference with drugs and biological constituents was assessed; no interferences were noted. Analysis of 100 random post-diagnostic urine specimens yielded 11 guanfacine positive results with concentrations ranging from 11 to 6390 ng/mL.

CONCLUSIONS

This HPLC-MS method provides a simple and rapid method for the routine detection and quantitation of guanfacine in urine specimens.

摘要

背景

胍法辛,一种用于治疗高血压的 α2-肾上腺素能激动剂(α2A),现正被用于治疗青少年的注意力缺陷多动障碍(ADHD)。这种新的治疗用途可能需要尿液检测来证明依从性或滥用。本文介绍了一种简单、快速的高效液相色谱-质谱(HPLC-MS)方法,用于检测和定量治疗后尿液中的胍法辛。

方法

胍法辛和普罗替林内标物从碱性尿液中用乙酸乙酯提取。有机层蒸发,用流动相重新配制,在 YMC Basic S-5 微米,2.0×150 毫米 HPLC 柱上分析,连接到正电喷雾电离模式的 MS 检测器,采用选择离子共振进行检测。洗脱时间<5 分钟。

结果

胍法辛的分析测量范围为 20-2000ng/mL。检测限和定量限分别为 5ng/mL 和 20ng/mL。在 40、100 和 500ng/mL(n=6)时,精度(%CV)<15%。使用相同浓度时的回收率>89%。对药物和生物成分的干扰进行了评估;未发现干扰。对 100 份随机诊断后尿液标本进行分析,有 11 份胍法辛阳性结果,浓度范围为 11-6390ng/mL。

结论

该 HPLC-MS 方法为尿液标本中胍法辛的常规检测和定量提供了一种简单、快速的方法。

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