HPLC/MS检测生物样品中的丁丙诺啡

Determination of buprenorphine in biological samples with high performance liquid chromatography-mass spectrometry

目的建立了生物样品中丁丙诺啡的高效液相色谱-电喷雾串联质谱检测方法。方法样品经固相萃取提取净化、反相液相色谱分离后进行质谱检测，根据保留时间及特征离子进行定性分析，以母离子m／z468进行定量分析。结果在10-500ng／ml（ng／g）范围内峰面积与质量浓度的线性关系良好（r^2〉0．993）。在50、100、500ng／ml（ng／g）3个添加水平，尿、血、肝中丁丙诺啡的平均回收率为74％～94％，日内测定结果的相对标准偏差小于8％，日间测定结果的相对标准偏差小于10％。结论该方法简单、灵敏，特异性强，适用于生物样品中丁丙诺啡的分析检验。

An analytical method for the determination of buprenorphine in biological samples was developed. In the procedure a solid-phase extraction for the isolation of Buprenorphine was employed, The samples were analyzed by reversed-phase high per formance liquid bromatograpby coupled with electrospray tandem mass spectrometry. The qualitative analysis was based on the retention time and fragment ions, and the quantitation was carried out with parent ion m/z 468. The linear ranges were from 10ng / ml（ng/g） to 500ng / ml（ng/g） and the correlation coefficients （r^2 ） were all greater than 0. 993. The average recoveries for Bu prenor-phine ranged from 74% to 94% in biological samples spiked with the drug concentrations of 50, 100 and 500ng / ml（ng/g）, and the relative standard deviations （RSDs ） were less than 8% for intra-day and 10% for inter-day determinations. The method is simple and suitable for the determination and confirmation of Buprenorphine in biological samples .