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目的建立醋酸艾塞那肽注射液主药及有关物质的含量测定方法。方法醋酸艾塞那肽含量测定采用TSK Gel G2000SW柱(300 mm×7.5 mm),检测波长为214 nm,流动相为水-乙腈-0.2 mol.L-1柠檬酸-三氟乙酸(体积比78∶17∶5∶0.2)。有关物质测定采用Polylc PolysulfoethylAsartamide色谱柱(100 mm×4.6 mm,3μm);梯度洗脱:流动相A为0.5 mol.L-1氯化钠与10 mmol.L-1磷酸二氢钠-乙腈(体积比56∶44,用磷酸调pH值至2.0),流动相B为10 mmol.L-1磷酸二氢钠-乙腈(体积比56∶44,用磷酸调pH值至2.0);检测波长为214 nm;流速为1 mL.min-1。结果醋酸艾塞那肽含量测定方法的检测限为0.1 ng,艾塞那肽质量浓度在0.052～1.04 g.L-1(r=0.999 8)内与峰面积呈良好线性关系,平均回收率为100.1%(n=9),RSD为0.77%,稳定性试验表明艾塞那肽溶液在室温条件下8 h内稳定。有关物质测定方法的检测限为2 ng,定量下限为5ng,专属性实验表明各杂质峰与主成分峰得到了有效的分离3,批样品的有关物质的含量检测结果分别为1.37%、1.64%1、.63%。结论本法快速、简便、分离效果较好,适用于醋酸艾塞那肽的含量测定及有关物质的质量控制。
Objective To establish a method for the determination of the main drug and related substances of exenatide acetate injection. Methods The determination of exenatide acetate was performed on a TSK Gel G2000SW column (300 mm × 7.5 mm) with a detection wavelength of 214 nm and a mobile phase of water - acetonitrile - 0.2 mol·L-1 citric acid - trifluoroacetic acid (volume ratio 78 : 17: 5: 0.2). The related substances were determined by Polylc PolysulfoethylAsartamide column (100 mm × 4.6 mm, 3 μm); gradient elution: mobile phase A was 0.5 mol·L -1 sodium chloride and 10 mmol·L -1 sodium dihydrogen phosphate-acetonitrile Than 56:44, adjusted to pH 2.0 with phosphoric acid), the mobile phase B was 10 mmol. L-1 sodium dihydrogen phosphate - acetonitrile (volume ratio of 56:44, adjusted to pH 2.0 with phosphoric acid); detection wavelength of 214 nm; flow rate was 1 mL.min-1. Results The detection limit of exenatide acetate was 0.1 ng. The exenatide showed a good linear relationship with the peak area in the range of 0.052-1.04 gL-1 (r = 0.999 8) with an average recovery of 100.1% (n = 9) with a RSD of 0.77%. Stability tests showed that exenatide was stable within 8 h at room temperature. The detection limit of the relevant substances is 2 ng, the lower limit of quantitation is 5 ng, and the specific experiments show that the impurity peaks and the main component peaks are effectively separated. The detection results of the related substances in batch samples are 1.37% and 1.64% 1, .63%. Conclusion The method is rapid, simple and has a good separation effect. It is suitable for the determination of exenatide acetate and the quality control of related substances.