色谱

色谱 ›› 2013, Vol. 31 ›› Issue (6): 572-576.DOI: 10.3724/SP.J.1123.2012.12013

• 研究论文 • 上一篇    下一篇

高效液相色谱-荧光检测法同时测定体外循环下狗血浆中的阿曲库铵和劳丹碱

杨莹莹1,4, 陈媚2, 邝毓姗3, 叶利明3, 张文胜4   

  1. 1. 山西省医药与生命科学研究院, 山西 太原 030006;
    2. 石家庄制药集团欧意药业有限公司, 河北 石家庄 050051;
    3. 四川大学华西药学院, 四川 成都 610041;
    4. 四川大学华西医院转化神经科学中心麻醉与危重急救研究室, 四川 成都 610041
  • 收稿日期:2012-12-05 修回日期:2013-01-18 出版日期:2013-06-28 发布日期:2013-06-06
  • 通讯作者: 张文胜

Determination of atracurium and laudanosine in dog plasma during cardiopulmonary bypass by high performance liquid chromatography with fluorometric detection

YANG Yingying1,4, CHEN Mei2, KUANG Yushan3, YE Liming3, ZHANG Wensheng4   

  1. 1. Shanxi Institute of Medicine and Life Sciences, Taiyuan 030006, China;
    2. Ouyi Pharma Co., Ltd., Shijiazhuang Pharmaceutical Group, Shijiazhuang 050051, China;
    3. West China School of Pharmacy, Sichuan University, Chengdu 610041, China;
    4. Laboratory of Anesthesia and Critical Care Medicine, Translational Neuroscience Center, West China Hospital, Sichuan University, Chengdu 610041, China
  • Received:2012-12-05 Revised:2013-01-18 Online:2013-06-28 Published:2013-06-06
  • Contact: 10.3724/SP.J.1123.2012.12013

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摘要：

建立了测定体外循环下狗血浆中阿曲库铵及其代谢产物劳丹碱的高效液相色谱-荧光检测(HPLC-FLD)分析方法。使用Agilent Eclipse Plus C18色谱柱分离,以0.03 mol/L磷酸氢二钾(pH 5.0)-乙腈(72:28, v/v)为流动相,流速1.0 mL/min。以维拉帕米为内标,样品经二氯甲烷萃取、浓缩后以流动相溶解进样,荧光检测的激发波长和发射波长分别为240和320 nm。结果表明,阿曲库铵和劳丹碱分别在25~5000 μ g/L和25~6000 μ g/L范围内线性关系良好(r=0.9990和r=0.9984);方法回收率在92.1%~109.5%之间;检出限分别为3 μ g/L和1 μ g/L;日内和日间精密度(以RSD计)均小于10%;稳定性试验结果显示样品在不同存储条件下的稳定性良好。该方法选择性好,灵敏度高,结果准确,重现性好,可用于阿曲库铵和劳丹碱的血药浓度测定及其药代动力学研究。

关键词: 阿曲库铵, 高效液相色谱, 狗血浆, 劳丹碱, 血药浓度, 荧光检测

Abstract:

A high performance liquid chromatographic method coupled with fluorometric detection has been developed for the determination of atracurium and its major metabolite laudanosine in dog plasma. The separation of atracurium and laudanosine was performed on an Agilent Eclipse Plus C18 column, and the mobile phase consisted of 0.03 mol/L dipotassium hydrogen phosphate and acetonitrile (72:28, v/v) at a flow rate of 1.0 mL/min. Verapamil was used as the internal standard. The sample was extracted by dichloromethane, concentrated and dissolved in the mobile phase. The detection is performed at 240 nm for excitation and 320 nm for emission. The results showed that the linear concentration ranges of the calibration curve were 25-5000 μ g/L for atracurium (r=0.9990), and 25-6000 μ g/L for laudanosine (r=0.9984). The recoveries were 92.1%-109.5%. The limits of detection were 3 μ g/L for atracurium and 1 μ g/L for laudanosine. The RSDs of intra-day and inter-day were less than 10%. The stability tests under various conditions have been performed. The method is specific, sensitive and accurate in the determination of atracurium and laudanosine, and also can be used for the pharmacokinetic investigations of atracurium and laudanosine in plasma.

Key words: atracurium, dog plasma, fluorometric detection (FLD), high performance liquid chromatography (HPLC), laudanosine, plasma concentration

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