离子色谱法测定血栓通注射液中辅料氯化钠和枸橼酸钠的含量

Determination of sodium chloride and sodium citrate of excipients in Xueshuantong injections by ion chromatography

目的：建立离子色谱法测定血栓通注射液中氯化钠、枸橼酸钠的含量。方法：采用AS-11-HC离子交换色谱柱（250 mm×4 mm）,AG-11-HC保护柱（50 mm×4 mm）,以35 mmol·L-1氢氧化钠溶液为流动相,等度洗脱,流速1.0 m L·min-1;阴离子抑制器,抑制电流90 m A;电导检测器,柱温30°;进样量100μL。对建立的方法进行线性范围、准确性以及精密度验证。结果：标准溶液中氯离子在1.0∽30.0μg范围内,氯离子色谱峰与其浓度呈良好的线性关系（r=1.000,n=6）,平均回收率为98.10%;标准溶液中枸橼酸根离子在0.5∽4.0μg范围内,枸橼酸根离子色谱峰与其浓度呈良好的线性关系（r=0.999 7,n=6）,平均回收率为102.9%;结果 5家企业13批样品均含有氯化钠,含量在7.407∽8.705 mg·m L-1;3家企业7批样品含有枸橼酸钠,含量在0.319∽1.157 mg·m L-1;2家企业均未检出枸橼酸钠。结论：本文设计方法经方法学验证可用于血栓通注射液中辅料氯化钠、枸橼酸钠的质量控制。

Objective ：To establish an ion chromatography hy method to determine the content of sodium chloride and sodium citrate in Xueshuantong injections. Methods：The established conditions for ion were as follows ：chroma- tographic column was IonPac AS-11 -HC （ 250 mm×4 mm） ; protect column was AG-11 -HC （ 50 mm×4 mm） ; mobile phase ： 35 mmol · L- 1 NaOH, time for isoeratic elution ; flow rate was 1.0 mL·min - 1 ; inhibitor was ASRS 4 mm anion inhibitor;inhibition current was 90 mA;detector：electrical conductivity detector column temperature was 30P ; sample loading was 100 μL. The developed method was determined for linear range, verified for accuracy and precision, and applied preliminarily. Results：The chromatographic peak area of reference showed good linear rela- tionship to chloridion ion concentration in the range of 1.0 -30.0 μg（ r = 1. 000 ,n = 6） ,the total mean recovery of chloridion ion was 98. 10% ;The citrate peak area of reference showed good linear relationship to citrate ion concen- tration was in the range of 0.5 - 4.0μg （ r = 0.999 7, n = 6 ） and the total mean of recovery citrate ion was 102.9%. The content of sodium chloride in 13 batches of samples from 5 factories was in the range of 7.407 - 8.705 mg· mL-l. The content of sodium citrate in 7 batches of samples from 3 factories was in the range of 0. 319 -1. 157 mg·mL-l and it was not detected in the samples from another 2 factories. Conclusion：The estab- lished method in this study can be used for content determination of sodium chloride and sodium citrate in Xueshuantong injections. It is simple, convenient and rapid, with high accuracy and precision by verification of method- ology. It can be used for quality control of sodium chloride and sodium citrate in Xueshuantong injections.