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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 a method for the determination of sodium chloride and sodium citrate in Xueshuantong Injection by ion chromatography. Methods: The mobile phase consisted of 35 mmol·L-1 sodium hydroxide solution with AS-11-HC column (250 mm × 4 mm) and AG-11-HC guard column (50 mm × 4 mm) Isocratic elution, flow rate 1.0 m L · min-1; Anion suppressor, inhibit current 90 m A; Conductivity detector, column temperature 30 °; Injection volume 100 μL. The established method is validated for linear range, accuracy and precision. Results: The calibration curve showed a good linearity (r = 1.000, n = 6) for the chloride ion in the standard solution within the range of 1.0 ~ 30.0μg with an average recovery of 98.10%. The standard solution of citrate ion In the range of 0.5 ~ 4.0μg, the citrate ion chromatogram showed a good linear relationship with the concentration (r = 0.999 7, n = 6), with an average recovery of 102.9%. Results The 13 batches of samples from five companies contained chlorination Sodium, the content of 7.407 ~ 8.705 mg · m L-1; 7 batches of three companies contain sodium citrate content of 0.319 ~ 1.157 mg · m L-1; two companies were not detected sodium citrate. Conclusion: This method is validated by methodological verification of Xueshuantong injection of sodium chloride, sodium citrate quality control.