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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 |
| 阅读数： | 1280 次 |
| 本月下载数： | 29 次 |
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