气相色谱-质谱法测定血浆中双氯芬酸钠的含量
GC-MS Determination of Sodium Diclofenac in Human Plasma
摘 要
提出了应用气相色谱-质谱法测定血浆中双氯芬酸钠含量.血浆样品中双氯芬酸钠经盐酸提取,并加入三甲基硅烷衍生化试剂进行衍生化,所得衍生化产物经萃取、净化后供气相色谱分离及质谱测定.采用选择离子质谱扫描方式,供试品双氯芬酸钠-三甲基硅烷衍生物定量选择离子检测质荷比为m/z 367,内标物布洛芬-三甲基硅烷衍生物定量选择离子检测质荷比为m/z 263.双氯芬酸钠的线性范围为0.005~5.0 mg·L-1,检出限(3S/N)为0.5 μg·L-1.方法回收率在94.6%~97.4%之间,日内、日间相对标准偏差(n＝6)均小于5%.
双氯芬酸钠
血浆
三甲基硅烷
GC-MS
Sodium diclofenac
Plasma
TMS
Abstract
The method of GC-MS was applied to the determination of sodium diclofenac in human plasma.The sample containing sodium diclofenac was acidified with HCl and derivatized with trimethylsilane.The derivatized product was extracted and purified,which was then used for GC-MS determination.The selected ion monitoring mode and values of m/z of 367 for diclofenac derivative and m/z of 263 for ibuprofen derivative (internal standrad) were adopted in the MS determination.Linearity range of sodium diclofenac was found between 0.005-5.0 mg·L-1,with detection limit (3S/N) of 0.5 μg·L-1.The values of recovery were found in the range of 94.6%-97.4%,with values of intraday and interday RSD′s less than 5%.
中图分类号 O657.63
所属栏目 工作简报
基金项目
收稿日期 2008/12/30
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备注余艳平(1982-),男,湖北黄冈人,硕士研究生,研究方向为药物分析.
引用该论文: YU Yan-ping,LIU Jun-ting,LI Ling,GAO Li-na,WANG Yan,SHENG Kai. GC-MS Determination of Sodium Diclofenac in Human Plasma[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(2): 153～155
余艳平,刘俊亭,李玲,高丽娜,王妍,盛开. 气相色谱-质谱法测定血浆中双氯芬酸钠的含量[J]. 理化检验－化学分册, 2010, 46(2): 153～155
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参考文献
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【4】LALA L G,D′MELLO P M,NAIK S R.HPTLC determination of diclofenac sodium from serum[J].J Pharm Biomed Anal,2002,29:539-540．
【5】阳利龙,祝文兵,张毕奎,等.固相萃取-HPLC法测定人血浆中双氯芬酸钠的浓度[J].中国药房,2007,18(8):594-596．
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【8】HAJ B M E,AINRI A M A,HASSAN M H,et al.The GC-MS analysis of some commonly used non-steriodal anti-inflammatory drugs (NSAIDs) in pharmaceutical dosage forms and in urine[J].Forensic Science International,1999,105:141-143．
【9】KAPHALIA L,KAPHALIA B S,KUMAR S,et al.Efficient high performance liquid chromatograph/ultraviolet method for determination of diclofenac and 4′-hydroxydiclofenac in rat serum[J].J Chromatogr B,2006,830:231-233．
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