摘要
目的:建立高效液相色谱法测定1种酰氯类化合物5-氯噻吩-2-甲酰氯。方法:采用Ameritech Accurasil C8(250 mm×4.6 mm,5μm)色谱柱,以0.01 mol·L^-1磷酸水溶液为流动相A,乙腈为流动相B进行梯度洗脱,流速1.0 mL·min^-1,柱温35℃,检测波长274 nm;以无水甲醇为衍生化试剂,三乙胺为缚酸剂,经衍生后进样测定。结果:5-氯噻吩-2-甲酰氯含量检测方法的专属性好;在1.012~2.040 mg·mL^-1浓度范围内线性良好r=0.9982,n=5;精密度、溶液稳定性好,RSD分别为0.040%(n=6)和1.2%(n=7);平均回收率(n=9)为99.0%,RSD为0.80%;色谱条件发生微小变化时,方法耐用性好;5-氯噻吩-2-甲酸的定量下限和检测下限分别为1.871μg·mL^-1和0.6237μg·mL^-1,5-氯噻吩-2-甲酰氯的定量下限和检测下限分别为1.562μg·mL^-1和0.4686μg·mL^-1;3批供试品中特定杂质和最大单一未知杂质含量均小于1.0%,主成分含量分别为98.5%、98.4%、98.4%。结论:本方法适用于5-氯噻吩-2-甲酰氯的测定,对于其他酰氯类化合物的测定也有重要的参考价值。
Objective:To establish an HPLC method for the determination of an acyl chloride compound 5-chlorothiophene-2-carbonyl chloride.Methods:HPLC was performed on an Ameritech Accurasil C8 column(250 mm×4.6 mm,5μm)with a gradient elution system of 0.01 mol·L^-1 phosphoric acid solution-acetonitrile.The flow rate was 1.0 mL·min^-1,and the column temperature was maintained at 35℃,the detection wavelength was 274 nm.Triethylamine and anhydrous methanol were added into the drug solution sequentially as acid binding and derivatization reagents,respectively.Results:The method had good specificity and it showed an excellent linearity within the range of 1.012-2.040 mg·mL^-1(r2=0.9982,n=5).The precision and solution stability were satisfactory,with the RSDs of 0.040%(n=6)and 1.2%(n=7),respectively.The average recovery was 99.0%,with the RSD of 0.80%(n=9).The method had good durability when chromatographic conditions changed slightly.The limit of quantitation of 5-chloro-2-thiophenecarboxylic acid and 5-chlorothiophene-2-carbonyl chloride were 1.871μg·mL^-1 and 1.562μg·mL^-1,respectively.The limit of detection of 5-chloro-2-thiophenecarboxylic acid and 5-chlorothiophene-2-carbonyl chloride were 0.6237μg·mL^-1 and 0.4686μg·mL^-1,respectively.The determination results of the three batches of samples showed that the contents of the specified impurity and the maximum single unknown impurity were less than 1.0%,and the contents of 5-chlorothiophene-2-carbonyl chloride were 98.5%,98.4%and 98.4%,respectively.Conclusion:The method is suitable for the determination of and it also has important reference value for the determination of other acyl chloride compounds.
作者
尹秀娥
陈阳
董乔
张嘉月
侯德粉
YIN Xiu-e;CHEN Yang;DONG Qiao;ZHANG Jia-yue;HOU De-fen(Shenyang SYRICI Festing Co.,Ltd.,Shenyang 110021,China;Liaoning Grand Nuokang Biopharmaceutical Co.,Ltd.,Shenyang 110171,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第11期2064-2069,共6页
Chinese Journal of Pharmaceutical Analysis
