建立全血中溴敌隆的固相萃取-液相色谱串联质谱联用检测方法。血液中加入pH=6缓冲溶液,用HLB固相小柱萃取浓缩后吹干,采用ZORBAX SB-C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,流动相为0.1%甲酸和20 m M乙酸铵-乙腈,流速为0.3 m L/min;...建立全血中溴敌隆的固相萃取-液相色谱串联质谱联用检测方法。血液中加入pH=6缓冲溶液,用HLB固相小柱萃取浓缩后吹干,采用ZORBAX SB-C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,流动相为0.1%甲酸和20 m M乙酸铵-乙腈,流速为0.3 m L/min;进样量:1μL,电喷雾离子源(ESI),负离子模式,采用多反应监测(MRM)监测。在50~800 ng/m L范围内线性良好,全血中溴敌隆在高中低三个浓度条件下的回收率为69.4%~72.2%,相对标准偏差为2.3%~5.0%;溴敌隆的仪器检出限为6.6 ng/m L。该固相萃取方法自动化高、溶剂用量少,可用于全血中的溴敌隆检测。展开更多
In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of an...In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of antibiotics and their related substances. In the first-dimensional chromatography, the analytes were separated on a zwitterion exchange-reversed phase-hydrophitic interaction （ZIC-RP-HILIC） mixed-mode column coupled with tandem mass spectrometry （LC-MS/MS）. A commonly used reversed phase LC column was employed in the second-dimensional chromatography. The mobile phase for the ZIC-RP-HILIC mixed-mode chromatography consisted of a volatile buffer that was compatible with LC-MS/MS, which enhanced the efficiency of ionization for structure elucidation. The antibiotic impurities eluted in the ion-pairing reversed phase chromatography were directly characterized by the ZIC-RP-HILIC-MS system, and the orthogonal separation of ZIC-RP-HILIC mixed-mode chromatography and reversed phase LC provided extra confidence that no impurity was missed. The efficiency of this method was demonstrated in the analysis of penicillin V potassium, oxacillin sodium, ceftriaxone sodium, and their impurities. In addition, this method is convenient for impurity profiling of antibiotics, and may be used for the analysis of other pharmaceutical ingredients.展开更多
基金The Key Projects in the National Science&Technology Pillar Program during the Twelfth Five-year Plan Period(Grant No.2012BAK25B02)
文摘In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of antibiotics and their related substances. In the first-dimensional chromatography, the analytes were separated on a zwitterion exchange-reversed phase-hydrophitic interaction （ZIC-RP-HILIC） mixed-mode column coupled with tandem mass spectrometry （LC-MS/MS）. A commonly used reversed phase LC column was employed in the second-dimensional chromatography. The mobile phase for the ZIC-RP-HILIC mixed-mode chromatography consisted of a volatile buffer that was compatible with LC-MS/MS, which enhanced the efficiency of ionization for structure elucidation. The antibiotic impurities eluted in the ion-pairing reversed phase chromatography were directly characterized by the ZIC-RP-HILIC-MS system, and the orthogonal separation of ZIC-RP-HILIC mixed-mode chromatography and reversed phase LC provided extra confidence that no impurity was missed. The efficiency of this method was demonstrated in the analysis of penicillin V potassium, oxacillin sodium, ceftriaxone sodium, and their impurities. In addition, this method is convenient for impurity profiling of antibiotics, and may be used for the analysis of other pharmaceutical ingredients.
