用高效液相色谱法分析血清中的纳曲酮及其代谢物6-β-纳曲醇。

Analysis of naltrexone and its metabolite 6-beta-naltrexol in serum with high-performance liquid chromatography.

作者信息

Heinälä Pekka, Lahti Tuuli, Sinclair David, Ariniemi Kari, Lillsunde Pirjo, Alho Hannu

机构信息

National Public Health Institute, Helsinki, Finland.

出版信息

BMC Res Notes. 2012 Aug 15;5:439. doi: 10.1186/1756-0500-5-439.

DOI:10.1186/1756-0500-5-439

PMID:22894733

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC3490825/

Abstract

BACKGROUND

Naltrexone has been proven to be an effective treatment option for the treatment of alcohol dependency. In this article we introduce a reliable and simple method developed for the simultaneous determination of naltrexone and 6-β-naltrexol in human serum by using high-performance liquid chromatography (HPLC).

FINDINGS

Liquid-liquid extraction with butyl acetate from basic solutions (pH 9) was chosen for extraction with nalorphine as an internal standard (IS). Analytes were back-extracted from organic solvent into perchloric acid. The acid extract was chromatographed by HPLC with a reverse-phase ODS-column and electrochemical detector. The mobile phase was a NaH(2)PO(4)-solution with acetonitrile as an organic modifier and octanesulphonic acid and tetraethylammonium hydrogen sulphate as ion-pair reagents. The recovery of the extraction method was 48% for naltrexone and 75% for 6-β-naltrexol. The limit of quantification was 5.0 ng/ml for naltrexone and 1.0 ng/ml for 6-β-naltrexol. The analysed concentrations of naltrexone differed from the theoretic concentrations by 0.7 to 2.3% and those of 6-β-naltrexol by 2.6%. The relative standard deviation of within-day assay was from 0.9 to 5.7% for naltrexone and from 0.8 to 4.2% for 6-β-naltrexol; for the between-day assay it was 5.7% and 4.2%, respectively.

CONCLUSIONS

Our results indicate that the developed method is suitable for determination of naltrexone and 6-β-naltrexol in human serum.

摘要

背景

纳曲酮已被证明是治疗酒精依赖的一种有效治疗选择。在本文中，我们介绍了一种通过高效液相色谱法（HPLC）同时测定人血清中纳曲酮和6-β-纳曲醇的可靠且简单的方法。

研究结果

选择用乙酸丁酯从碱性溶液（pH 9）中进行液液萃取，以烯丙吗啡作为内标（IS）。分析物从有机溶剂中反萃取到高氯酸中。酸提取物通过HPLC用反相ODS柱和电化学检测器进行色谱分析。流动相是含有乙腈作为有机改性剂以及辛烷磺酸和硫酸氢四乙铵作为离子对试剂的磷酸二氢钠溶液。该萃取方法对纳曲酮的回收率为48%，对6-β-纳曲醇的回收率为75%。纳曲酮的定量限为5.0 ng/ml，6-β-纳曲醇的定量限为1.0 ng/ml。分析的纳曲酮浓度与理论浓度相差0.7%至2.3%，6-β-纳曲醇的浓度相差2.6%。日内测定的相对标准偏差对于纳曲酮为0.9%至5.7%，对于6-β-纳曲醇为0.8%至4.2%；日间测定的相对标准偏差分别为5.7%和4.2%。