关锋,武小锋,孙承程,刘有平,邸欣
GUAN Feng,WU Xiao-feng,SUN Cheng-cheng,LIU You-ping,DI Xin

• 1:沈阳药科大学药学院
• 2:辽宁爱母医疗科技有限公司

摘要(Abstract)：

目的建立快速、灵敏的液相色谱-大气压化学电离-串联质谱(LC-APCI-MS/MS)法测定植入含药宫内节育器(IUD)后Beagle犬血浆中的吲哚美辛质量浓度。方法血浆样品经乙腈沉淀蛋白后,采用Diamonsil C18柱(150 mm×4.6 mm,5μm)分离,流动相为甲醇-乙腈-水-甲酸(体积比为45∶45∶10∶0.5),流速为0.45 mL·min-1。采用大气压化学电离(APCI)源,以选择反应监测(SRM)方式进行检测,用于定量分析的离子反应分别为m/z 358→m/z 111(吲哚美辛)和m/z 419→m/z343(内标,尼莫地平)。结果血浆中吲哚美辛的线性范围为1.0~200.0μg·L-1,定量下限为1.0μg·L-1,提取回收率为83.3%~91.4%,日内精密度不大于9.8%,日间精密度不大于5.9%,准确度(RE)在93.6%~100.0%内。结论该法简便、快速、灵敏,适用于植入含吲哚美辛的IUD的Beagle犬血浆中吲哚美辛的测定。
Objective To develop and validate a rapid and sensitive liquid chromatography-tandem mass spectrometric( LC-MS / MS) method for measuring plasma levels of indomethacin in Beagle dogs after insertion of intrauterine device(IUD). Methods Indomethacin and internal standard w ere extracted from plasma w ith acetonitrile and separated on a Kromasil C18column using a mobile phase consisting of methanol,acetonitrile,w ater and formic acid( V ∶ V ∶ V ∶ V = 45 ∶ 45 ∶ 10 ∶ 0. 5) at a flow rate of 0. 45 mL·min- 1. Mass spectrometric detection w as achieved by a triple-quadrupole mass spectrometer equipped w ith an atmospheric pressure chemical ionization source( APCI) operating in positive ionization mode. Selected reaction monitoring(SRM) using the precursor-product ion transitions of m / z 358→m/z 111 and m/z 419→m/z 343 were performed to quantify indomethacin and internal standard( nimodipine),respectively. Results The assay w as linear over the concentration range of 1. 0-200. 0 μg·L- 1for indomethacin. The low er limit of quantification( LLOQ) was 1. 0 μg·L- 1. The extraction recovery w as more than 83. 3%. The intra-day and inter-day precision w ere less than 9. 8% and 5. 9%,respectively. The accuracy w as w ithin 93. 6%-100. 0%. Conclusions The method is simple,rapid and sensitive,and can be successfully applied to determine indomethacin in Beagle dogs plasma after insertion of IUD.

关键词(KeyWords)： 吲哚美辛;宫内节育器;高效液相色谱串联二级质谱法;Beagle犬;血浆
indomethacin;IUD;LC-MS /MS;Beagle dog;plasma

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 关锋,武小锋,孙承程,刘有平,邸欣
GUAN Feng,WU Xiao-feng,SUN Cheng-cheng,LIU You-ping,DI Xin

DOI: 10.14066/j.cnki.cn21-1349/r.2013.11.010

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