HPLC法测定乙酰半胱氨酸泡腾片的对映异构体含量

Determination of the Enantiomers in Acetylcysteine Effervescent Tablets by HPLC

建立一个可检测乙酰半胱氨酸泡腾片中对映异构体含量的方法。采用CHIRALPAK AY-H手性色谱柱(250 mm×4.6mm,5μm);以正己烷-无水乙醇-三氟乙酸(90∶10∶0.1)为流动相,等度洗脱;柱温为20℃;流速为1.0 m L·min^(-1);检测波长为216 nm。在所选定的液相色谱条件下,乙酰半胱氨酸峰与其对映异构体峰分离良好,辅料峰均不干扰对映异构体的检测;最低检测限为12.7 ng;12份加标供试品溶液的重复性结果RSD为1.9%;对映异构体的浓度在1.4879~8.9272μg·m L^(-1)范围内与峰面积呈良好的线性关系(r=0.9999);微小改变流速、柱温与流动相比例等色谱条件,对检测结果均无影响。该方法专属性强、灵敏度与精密度高,耐用性良好,可用于测定乙酰半胱氨酸泡腾片中的对映异构体含量。

To establish a method for the determination of enantiomers in acetylcysteine effervescent tablets.The CHIRALPAK AY-H(250 mm×4.6 mm,5μm)chiral column was used.Mobile phase was n-hexane-absolute ethanol-trifluoroacetic acid(90∶10∶0.1)with equal elution.The column temperature was 20℃.The flow rate was 1.0 mL·min^(-1).The detection wavelength is 216 nm.Under the selected conditions of liquid chromatography,the peaks of acetylcysteine and enantiomers were separated well,and the excipients did not interfere with the detection of enantiomers.The limit of detection was 12.7 ng.The RSD of 12 samples was 1.9%.The concentration of enantiomers showed a good linear relationship with the peak area in the range of 1.4879μg·mL^(-1) to 8.9272μg·mL^(-1)(r=0.9999).Slightly changed the chromatographic conditions,such as flow rate,column temperature and mobile phase ratio,had no effect on the detection results.The method has strong specificity,high sensitivity,high precision and good robustness,and can be used for the determination of enantiomers in acetylcysteine effervescent tablets.