HPLC法测定对乙酰氨基酚片中有关物质的含量
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篇名: HPLC法测定对乙酰氨基酚片中有关物质的含量
TITLE: Content Determination of Related Substances in Paracetamol Tablets by HPLC
摘要: 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Agilent5HC-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0.9mL/min,检测波长为254nm,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≥0.9998),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0.0096、0.0242、0.1640、0.0511、0.0559、0.4220ng,定量限分别为0.0320、0.0806、0.5460、0.1700、0.1860、1.4060ng;平均回收率为95.96%~111.09%(RSD为0.05%~2.42%);精密度试验的RSD均小于15%,且耐用性良好。3批样品均检出了对氨基酚(均为0.006%)、杂质B(0.016%~0.017%)、未知杂质(0.0020~0.0021%),未检出对氯苯乙酰胺和杂质A、D、F。结论:该方法专属性强、准确度高,可用于对乙酰氨基酚片有关物质的测定。
ABSTRACT: 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 5HC-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 5 μL. 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, 0.246-18.462 μg/mL(r≥0.999 8),respectively. Correction factors of impurity A ,B,D,F were 2.9,1.0,1.2,6.2. The limits of detection were 0.009 6,0.024 2,0.164 0,0.051 1,0.055 9,0.422 0 ng;the limits of quantitation were 0.032 0,0.080 6,0.546 0,0.170 0,0.186 0,1.406 0 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(0.002 0%-0.002 1%)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.
期刊: 2020年第31卷第10期
作者: 杨莉,梅勇,龙涛,罗磊,陈小雪
AUTHORS: YANG Li,MEI Yong,LONG Tao,LUO Lei,CHEN Xiaoxue
关键字: 高效液相色谱法;对乙酰氨基酚片;有关物质;含量
KEYWORDS: HPLC;Paracetamol tablets ;Related substance ;Content
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