全自动柱切换高效液相色谱系统测定人血浆中奥卡西平的浓度

目的采用全自动柱切换HPLC系统建立人血浆中奥卡西平的测定方法,用于临床治疗药物监测。方法全自动柱切换HPLC由萃取色谱系统及分析色谱系统2个部分构成,萃取柱为ASTON-RG C8柱(4.6 mm×50 mm,5μm,ANAX),分析柱为ASTON-RG C18柱(4.6 mm×250 mm,5μm,ANAX);2个系统间通过"中心切割"模式进行目标物转移,转移时间窗口2.6～4.2 min;聚焦流速为2.0 mL min-1,聚焦时间为0～0.6 min;检测波长305 nm;进样量100μL;采用外标法计算结果。结果标准曲线在0.47～26.07μg mL-1呈良好线性关系,相关系数为0.999 6,最低检测限为0.12μg mL-1,低(1.42μg mL-1)、中(11.85μg mL-1)、高(26.07μg mL-1)浓度的绝对回收率为95.6%～98.9%,日内和日间精密度均<5.0%,准确度99.6%～102.7%。结论本方法抗干扰能力强、自动化程度高、准确度和灵敏度高等优点,适合奥卡西平治疗药物监测的常规应用。

柱切换高效液相色谱法测定抗病毒口服液中连翘苷、靛蓝及靛玉红的含量

目的:柱切换高效液相色谱法测定抗病毒口服液中连翘苷、靛蓝及靛玉红的含量。方法:采用 Alltima C_(18)分析柱(200mm×4.6mm),流动相:甲醇-磷酸盐缓冲液(pH=5;53:47),检测波长280nm,流速1mL·min^(-1),柱温20℃。结果:连翘苷、靛蓝及靛玉红分别在2.08～20.82μg·mL^(-1)(r=0.9999),2.82～28.16μg·mL^(-1)(r=0.9999)和3.02～30.20μg·mL^(-1)(r=0.9999)范围内呈线性。连翘苷、靛蓝及靛玉红的加样回收率分别为99.4%(RSD=1.0%),101.7%(RSD=0.8%)和101.8%(RSD:1.6%)。结论:实验简便,可靠,对控制药品质量及提高标准提供一个参考方法。

CS-HPLC法测定抗病毒口服液中连翘苷、靛蓝及靛玉红的含量

目的:柱切换高效液相色谱法测定抗病毒口服液中连翘苷、靛蓝及靛玉红的含量.方法:采用Alltima C18分析柱(200mm×4.6mm),流动相:甲醇-磷酸盐缓冲液(pH=5;53:47),检测波长280nm,流速1ml·min-1,柱温20℃.结果:连翘苷、靛蓝及靛玉红分别在2.08～20.82μg·ml-1(r:0.9999)、2.82～28.16μg·ml-1(r:0.9999)和3.02～30.20μg.ml-1(r:0.9999)范围内呈线性.连翘苷、靛蓝及靛玉红的加样回收率分别为99.4%(RSD:1.0%)、101.7%(RSD为0.8%)和101.8%(RSD:1.6%).结论:实验简便,可靠,对控制药品质量及提高药品质量标准提供一个参考方法.

Determination of Lansoprazole by Direct Injection of Plasma and High Performance Liquid Chromatography with Column Switching

High performance liquid chromatography with column switching has been developed for the determination of lansoprazole in plasma. The plasma samples were injected onto a pretreatment column packed with LiChromprep RP2 (25～40 mm) after simple dilution with distilled water. Distilled water was used to wash out protein and other polar components in plasma. After switching, the concentrated lansoprazole was eluted in the backflush mode onto a Shimpack CLC ODS column with methanol 0 2 mol·L 1 ammonium acetate (65:35) as mobile phase. Purge solutions were used for clean up and for regenerating the pretreatment column. The method showed good precision and recovery. The detection limit was 0 005 mg·L -1 plasma. The RSD’s (intra and interday) were less than 2 5% and 5 3% respectively. The method has been successfully used to determine pharmacokinetics of lansoprazole in Chinese volunteers.

Combination of reversed phase liquid chromatography and zwitterion exchange-reversed phase-hydrophilic interaction mixed-mode liquid chromatography coupled with mass spectrometry for the analysis of antibiotics and their impurities

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.