Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Hradec Králové, Czech Republic.
Electrophoresis. 2011 Apr;32(8):890-5. doi: 10.1002/elps.201000456. Epub 2011 Mar 10.
A novel capillary electrophoretic method for the separation of pancuronium (PM) and vecuronium (VM) ions utilizing capacitively coupled contactless conductivity detection was devised and validated. The separation was carried out in bare fused-silica capillaries (50 μm id, 75/45 cm) at 25°C. Optimal BGE was 50 mM borate buffer of pH 9.5 containing 12.5 mg/mL of (2-hydoxypropyl)-γ-CD. The samples were injected hydrodynamically at 1000 mbar for 3 s. Separation was performed at +30 kV. Under such conditions the PM and VM were base-line resolved and the separation took < 4 min. For quantification phenyltrimethylammonium iodide was used as internal standard. Calibration curves were linear for both pancuronium bromide (PMB) and vecuronium bromide (VMB) in the range 25-250 μg/mL with r> 0.9968. The limits of detection were 7 and 6 μg/mL for PMB and VMB, respectively. The accuracy tested by recovery experiment at three concentration levels of added PMB and VMB was satisfactory (95.7-102.7%, n =3, with RSD < 2.61%). The method was successfully applied to the assay of PMB and VMB in commercial injection solutions.
设计并验证了一种新的毛细管电泳分离方法,用于分离泮库溴铵(PM)和维库溴铵(VM)离子,利用电容耦合非接触式电导检测。在 25°C 下,在裸熔融硅毛细管(50 μm id,75/45 cm)中进行分离。最佳 BGE 为 50 mM 硼酸缓冲液,pH 值为 9.5,其中含有 12.5 mg/mL 的(2-羟丙基)-γ-CD。样品以 1000 mbar 的压力在 3 s 内进行水力注射。在+30 kV 的条件下进行分离。在此条件下,PM 和 VM 实现了基线分离,分离时间<4 分钟。对于定量分析,使用苯扎三甲基溴化铵作为内标。在 25-250 μg/mL 的范围内,对泮库溴铵溴化物(PMB)和维库溴铵溴化物(VMB)进行校准曲线线性拟合,相关系数 r>0.9968。PMB 和 VMB 的检测限分别为 7 和 6 μg/mL。通过在三个添加 PMB 和 VMB 的浓度水平进行回收实验测试的准确性令人满意(95.7-102.7%,n=3,RSD<2.61%)。该方法成功应用于商业注射溶液中 PMB 和 VMB 的测定。