| 高效液相色谱-四极杆/线性离子阱质谱仪测定盐酸黄酮哌酯中的1-(2-羟乙基)哌啶残留 |
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| 基金项目:国家质检总局科技计划项目(2015QK165) |
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| 中文摘要:建立了盐酸黄酮哌酯中1-(2-羟乙基)哌啶的高效液相色谱-四极杆/线性离子阱质谱(HPLC-QTRAP-MS/MS)定量分析方法。盐酸黄酮哌酯药物用0.1%甲酸溶解后，经Agilent ZORBAX SB-Aq C18(2.1 mm×100 mm，1.8 μm)色谱柱分离，以乙腈-0.1%甲酸水作为流动相进行梯度洗脱，采用电喷雾正离子扫描方式，以选择反应监测(SRM)模式进行检测。结果表明，1-(2-羟乙基)哌啶在10~100 μg/L范围内线性关系良好(r=0.999 7)，加标回收率为98.9%~1068%，相对标准偏差(RSD)均不大于3.0%，方法检出限(S/N=3)为6.0 mg/L，方法定量下限(S/N=10)为20 mg/L。该方法简单、灵敏、准确，适用于盐酸黄酮哌酯中1-(2-羟乙基)哌啶残留的测定。 |
| 中文关键词:高效液相色谱-四极杆/线性离子阱质谱仪 盐酸黄酮哌酯 1-(2-羟乙基)哌啶 |
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| Determination of 1-(2-Hydroxyethyl)piperidine in Flavoxate Hydrochloride by HPLC-QTRAP-MS/MS |
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| Abstract:A high performance liquid chromatography-quadrupole ion trap tandem mass spectrometric(HPLC-QTRAP-MS/MS) method was developed for the quantification of 1-(2-hydroxyethyl) piperidine residue in flavoxate hydrochloride.After dissolved with 0.1% formic acid,the flavoxate hydrochloride sample was loaded onto an Agilent ZORBAX SB-Aq C18(2.1 mm×100 mm，1.8 μm) column to separate with a mobile phase of 0.1% formic acid-acetonitrile.The electrospray was operated in positive ion mode,and the sample was monitored in the select reaction monitoring(SRM) mode.As a result,the calibration curve of 1-(2-hydroxyethyl)piperidine showed a good linearity(r=0.999 7) in the range of 10-100 μg/L.The recoveries were in the range of 98.9%-106.8%,with relative standard deviations(RSDs) not more than 3.0%.The limit of detection(LOD,S/N=3) for the method was 6.0 mg/L,and the limit of quantitation(LOQ,S/N=10) was 20 mg/L.The method has the advantages of simple operation,high sensitivity and good reproducibility,and could be used for the detection of 1-(2-hydroxyethyl)piperidine in flavoxate hydrochloride. |
| Key Words:high performance liquid chromatography-quadrupole ion trap tandem mass spectrometry(HPLC-QTRAP-MS/MS) flavoxate hydrochloride 1-(2-hydroxyethyl)piperidine |
| 引用本文：许洁,周长朋，郑文凤，王春玲.高效液相色谱-四极杆/线性离子阱质谱仪测定盐酸黄酮哌酯中的1-(2-羟乙基)哌啶残留[J].分析测试学报,2017,36(7):906-910. |
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