LC-MS/MS法测定阿片依赖者尿中丁丙诺啡及其代谢物和纳诺酮浓度 |
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引用本文: | 刘霞,倪晓佳,尚德为,张明,胡晋卿,王占璋,邱畅,温预关.LC-MS/MS法测定阿片依赖者尿中丁丙诺啡及其代谢物和纳诺酮浓度[J].广东医药学院学报,2014(2):136-141. |
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作者姓名: | 刘霞 倪晓佳 尚德为 张明 胡晋卿 王占璋 邱畅 温预关 |
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作者单位: | [1]广州医科大学附属脑科医院药学部,广东广州510370 [2]山东省交通医院药剂科,山东济南250031 |
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基金项目: | 广东华南药物临床试验公共服务平台建设/广东省重大科技专项立项资助(2011A080300003);国家临床重点专科资助项目(20121007);广东省药学会医院药学研究基金(奥赛康基金)(2013A12) |
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摘 要: | 目的 建立简单、快速的LC-MS/MS法,用于测定阿片依赖者尿中丁丙诺啡及其代谢物N-去烷基丁丙诺啡和纳诺酮的浓度,并进行尿排泄动力学研究.方法 尿样经NaOH碱化后进行液液萃取,丁丙诺啡以曲马多为内标、正己烷进行提取,N-去烷基丁丙诺啡和纳诺酮则以纳美芬为内标、乙酸乙酯-二氯甲烷(体积比4∶1)进行提取;质谱检测采用正离子模式,电喷雾离子化,多反应监测方式测定样品浓度;12名阿片依赖者口服复方丁丙诺啡纳诺酮舌下片4片(丁丙诺啡8 mg∶纳洛酮2 mg),计算尿中排泄率和尿药动力学参数,以考察排泄情况.结果 丁丙诺啡、N-去烷基丁丙诺啡和纳诺酮的线性范围分别为0.05 ~ 20 μg/L、1 ~ 200 μg/L和1~ 500 μg/L,定量下限分别为0.05 μg/L、1μg/L和1μg/L,提取回收率均大于76%,日内、日间RSD均小于8.4%;尿中排泄率分别为0.90%、2.13%和30.01%.结论 该法简单、快速、专属性强、重复性好,可用于阿片依赖者尿中丁丙诺啡、N-去烷基丁丙诺啡和纳诺酮浓度测定及排泄药动学研究.
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关 键 词: | 丁丙诺啡N-去烷基丁丙诺啡 纳诺酮 LC-MS MS 排泄动力学 |
Determination of buprenorphine and its metabolite and naloxone in urine from opioid-dependent subjects by LC-MS/MS |
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Authors: | LIU Xia NI Xiaojia SHANG Dewei ZHANG Ming HU Jinqing WANG Zhanzhang QIU Chang WEN Yuguan |
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Institution: | 1. Department of Pharmacy, Guangzhou Brain Hospital, Guangzhou Medical University, Guangzhou 510370, China ; 2. Department of Pharmacy, Shandong Jiaotong Hospital, Jinan 250031, China) |
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Abstract: | Objective To develop a simple and rapid LC-MS/MS method for the determination of buprenorphine and its metabolite norbuprenorphine (NBUP) and naloxone in urine from opioid-dependent subjects and study its excretion pharmacokinetics. Methods After urine alkalified, buprenorphine and internal standard (IS) were extracted with n-hexane, while acetic ether: dichlommethane ( 4 : 1 ) were used for norbuprenorphine, naloxone and IS, respectively. Positive ion mode was used with multiple reactions monitoring (MRM) by using electrospray ionization (ESI). Excretion rates were studied in 12 opioid- dependent subjects after oral administration of four compound buprenorphine naloxone sublingual tablets (buprenorphine 8 mg: naloxone 2 mg).Results The calibration curves of buprenorphine, norbuprenorphine and naloxone were linear ranging from 0.05-20 μg/L, 1- 200 μg/L, and 1- 500 μg/L.The lower limit of quantification were 0.05 μg/L, 1 μg/L and 1 μg/L. The recoveries were more than 76%.The intra and inter-day precision were less than 8.4%.Excretion rates were 0.90%,2.13% and 30.01%, respectively. Conclusion The method is simple, rapid, and accurate, which can be applied to determine buprenorphine, norbuprenorphine and naloxone concentration in urine and excretion pharmacokinetics. |
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Keywords: | buprenorphine norbuprenorphine naoxone LC-MS/MS excretion pharmacokinetics |
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