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目的建立高效阴离子交换色谱积分脉冲安培检测法同时测定门冬氨酸钾镁葡萄糖注射液中门冬氨酸和葡萄糖的含量。方法采用CarboPacTM PA20阴离子分离柱(3 mm×250 mm)和PA20保护柱(3 mm×50 mm);以去离子水为淋洗液A、200 mmol/L的氢氧化钠溶液为淋洗液B、1 mol/L的醋酸钠为淋洗液C,进行梯度洗脱,流速为0.5 ml/min;积分脉冲安培检测器(金工作电极、pH-Ag/Agcl参比电极);检测器温度30℃;柱温30℃,进样量25μl。结果葡萄糖和门冬氨酸两种成分线性范围分别为0.7952μg/ml~25.4470μg/ml(r=0.9996)和0.1122μg/ml~7.1808μg/ml(r=0.9998);葡萄糖和门冬氨酸两种成分高、中、低3种浓度的回收率分别在98.77%~100.14%之间和98.15%~100.05%之间,相对标准偏差分别为0.6%(n=9)和0.5%(n=9)。结论该法操作简便、专属性强、门冬氨酸和葡萄糖的分离效果好,可用于门冬氨酸钾镁葡萄糖注射液中门冬氨酸和葡萄糖的含量测定。
OBJECTIVE To establish a high performance anion exchange chromatography with integrated pulse amperometry for the simultaneous determination of aspartate and glucose in aspartate potassium and magnesium dextrose injection. Methods CarboPacTM PA20 anion column (3 mm × 250 mm) and PA20 guard column (3 mm × 50 mm) were used. With deionized water as eluent A and 200 mmol / L sodium hydroxide as eluent B , 1 mol / L sodium acetate as eluent C, gradient elution at a flow rate of 0.5 ml / min; integrated pulse amperometric detector (gold working electrode, pH-Ag / Agcl reference electrode); detector temperature 30 ℃; column temperature 30 ℃, injection volume 25μl. Results The linear ranges of glucose and aspartate were 0.7952μg / ml ~ 25.4470μg / ml (r = 0.9996) and 0.1122μg / ml ~ 7.1808μg / ml The recoveries of high, middle and low concentrations of two components were between 98.77% and 100.14% and between 98.15% and 100.05% with relative standard deviations of 0.6% (n = 9) and 0.5% (n = 9). Conclusion The method is simple, specific and strong, aspartic acid and glucose separation effect is good, can be used for determination of aspartic acid and glucose in potassium and magnesium aspartate glucose injection.