摘要:
This study was aimed to establish a method for simultaneous determination of seven anions and organic acids in Huo-Xue Tong-Luo (HXTL) injection by HPCE. With tartaric acid as the internal standard, separation was performed on an uncoated fused silica capillary (50 μm × 64. 5 cm, 56 cm of effective length). The 14 mmol·L-1 potassium acid phthalate and 0.1 mmol·L-1 hexadecyl trimethyl ammonium chloride were selected for the running buffer solution (pH 5.6). The separation voltage was -16 kV. The detection wavelength was set at 210 nm. The column temperature was maintained at 25 °C . The sample was injected at 50 mbar×4 s. The results showed that calibration curves of chloride ion, sulfuric acid root ion, formate ions, malic acid, succinic acid, iodate ion and acetic acid ions showed good linear relationship 41.4-248.2 μg·mL-1 (r = 0.999 3), 12.5-74.8 μg·mL-1 (r = 0.999 8), 18.2-109.1 μg·mL-1 (r = 0.999 8), 20.3-121.6 μg·mL-1 (r = 0.999 5), 17.2-103.1 μg·mL-1 (r=0.999 1), 17.6-105.6μg·mL-1 (r=0.999 6), 51.6-309.6μg·mL-1 (r=0.999 7), respectively. The average recoveries were 102.6%, 97.3%, 102.2%, 99.0%, 99.2%, 97.8%, and 103.4%, respectively. The RSD were 1.7%, 2.0%, 1.6%, 2.6%, 2.1%, 2.9%, and 1.0%, respectively (n = 6). It was concluded that the method was accurate and reproducible. It was suitable for the determination of anions and organic acids in HXTL injection.%目的:建立同时测定注射用活血通络中阴离子及有机酸等7种成分含量的方法。方法:采用HPCE法,以酒石酸为内标,Agilent未涂层石英毛细管柱(50μm×64.5 cm,有效长度56 cm)为分离通道;含14 mmol·L-1邻苯二甲酸氢钾及0.1 mmol·L-1十六烷基三甲基氯化铵的溶液(pH5.6)为运行缓冲液;分离电压为-16 kV,检测波长为210 nm,毛细管温度为25°C,压力进样50 mbar×4 s。结果:氯离子、硫酸根离子、甲酸根离子、苹果酸、丁二酸、碘酸根离子、乙酸根离子7种成分分别在41.4-248.2μg·mL-1(r=0.9993),12.5-74.8μg·mL-1(r=0.9998),18.2-109.1μg·mL-1(r=0.9998),20.3-121.6μg·mL-1(r=0.9995),17.2-103.1μg·mL-1(r=0.9991),17.6-105.6μg·mL-1(r=0.9996),51.6-309.6μg·mL-1(r=0.9997)浓度范围内呈现良好线性关系;平均回收率分别为102.6%、97.3%、102.2%、99.0%、99.2%、97.8%、103.4%, RSD分别为1.7%、2.0%、1.6%、2.6%、2.1%、2.9%、1.0%(n=6)。结论:该方法准确可靠,重复性良好,可用于注射用活血通络中阴离子及有机酸的含量测定。