HPLC法测定对乙酰氨基酚片中有关物质的含量

目的:建立测定对乙酰氨基酚片中有关物质含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent 5HC-C8,流动相A、B分别为甲醇-水-冰醋酸(50∶950∶1,V/V/V)和甲醇-水-冰醋酸(500∶500∶1,V/V/V)(梯度洗脱),流速为0.9 m L/min,检测波长为254 nm,柱温为40℃,进样量为5μL。结果:该色谱条件下,对乙酰氨基酚片中的主药(对乙酰氨基酚)、6个已知杂质(对氨基酚、对氯苯乙酰胺和杂质A、B、D、F)、3个制剂特定辅料(羟苯甲酯、羟苯乙酯和羟苯丙酯)和1个未知杂质的分离度均大于1.5。6个已知杂质检测质量浓度的线性范围分别为0.539～1.617、0.026～0.384、0.237～17.799、0.257～19.271、0.239～17.955、0.246～18.462μg/mL(r≥0.999 8),杂质A、B、D、F的校正因子分别为2.9、1.0、1.2、6.2;检测限分别为0.009 6、0.024 2、0.164 0、0.051 1、0.055 9、0.422 0 ng,定量限分别为0.032 0、0.080 6、0.546 0、0...

Content Determination of Related Substances in Paracetamol Tablets by HPLC

OBJECTIVE:To establish the method for content determination of related substances in Paracetamol tablets.METHODS:HPLC method was adopted.The determination was performed on Agilent 5 HC-C8 column with mobile phase A consisted of methanol-water-glacial acetic acid(50∶950∶1,V/V/V)and mobile phase B consisted of methanol-water-glacial acetic acid(500∶500∶1,V/V/V)(gradient elution)at the flow rate of 0.9 mL/min.The detection wavelength was set at 254 nm,and column temperature was 40℃.The sample size was 5μL.RESULTS:Under the chromatographic condition,the resolutions of main component(paracetamol),6 known impurities(p-aminophenol,p-chloroacetanilide,impurity A,B,D,F),3 specific excipients(methyl hydroxybenzoate,ethyl hydroxybenzoate,propyl hydroxybenzoate)and 1 unknown impurity were all higher than 1.5.The linear range of 6 known impurities were 0.539-1.617,0.026-0.384,0.237-17.799,0.257-19.271,0.239-17.955,0.246-18.462μg/mL(r≥0.9998),respectively.Correction factors of impurity A,B,D,F were 2.9,1.0,1.2,6.2.The limits of detection were 0.0096,0.0242,0.1640,0.0511,0.0559,0.4220 ng;the limits of quantitation were 0.0320,0.0806,0.5460,0.1700,0.1860,1.4060 ng.Average recoveries were 95.96%-111.09%(RSDs were 0.05%-2.42%).The RSDs precision test were low than 15%,and the durability were good.p-aminophenol(all were 0.006%),impurity B(0.016%-0.017%)and unknown impurity(0.0020%-0.0021%)were detected in 3 batches of sample.p-choroacetanilide,impurity A,D and F were not detected.CONCLUSIONS:The method is specific,accurate and suitable for the determination of related substance in Paracetamol tablets.