天麻胶囊质量标准中补充检验对乙酰氨基酚的方法

Method for supplemental test of paracetamol in quality standard of Tianma capsules

目的:建立检查"天麻胶囊中添加对乙酰氨基酚"的补充检验方法。方法:采用TLC法进行快速筛查;采用HPLC-PDA法进行定量检验,色谱柱为Polaris C18(4.6 mm×250 mm,5μm),流动相为甲醇-0.6%醋酸(10∶90),流速为1.0 mL.min-1,检测波长为243 nm,柱温为30℃;采用IR法进行快速鉴别;采用UPLC-MS法进行结构确认,色谱柱为Acquity UPLCBEHC18(50 mm×2.1 mm×1.7μm),流动相为0.1%甲酸-乙腈(5∶95),流速为0.4 mL.min-1。质谱条件采用正离子检测,电喷雾电离源(ESI),源电压为3.1 kV,毛细管温度为400℃,锥孔电压为30 V,鞘气流速为600 L.h-1,采用一级全扫描及二级全扫描方式,质量范围50～1000。结果:TLC法简便快速,专属性强,可作为非法添加的快速初筛;HPLC-PDA法可准确检验所添加对乙酰氨基酚的含量,所测5批样品中有3批检出,2批未检出;UPLC-MS法进行结构确认,特征性强,准确度高。结论:该方法适用于中成药中检测非法加入的对乙酰氨基酚成分,确证性强,灵敏度高。

Objective：To establish a supplemental test method to identify illegally added paracetamol in Tianma capsules. Methods： Rapid screening was performed by TLC method. HPLC - PDA was adopted to conduct the quan-titative inspection,the column was Polaris Cls （4.6 mm×250 mm,5μm）,the mobile phase was methanol - 0. 6% acetic acid （10： 90）at a flow rate of 1.0 mL min^-1 with a detection wavelength of 243 nm,the column tem-perature was 30 ℃. IR method was used for rapid identification with UPLC - MS method for the structural confirma-tion;the column was Acquity UPLC BEH C1s（50 mm×2.1 mm×1.7μm） ,the mobile phase was 0. 1% for-mic acid - acetonitrile （5： 95） at a flow rate of 0. 4 mL · min^ - 1. Mass conditions were set in a positive ion mode for detection with electrical ionization source （ESI） , the source voltage of 3.1 kV, the capillary temperature of 400 ℃, the cone voltage of 30 V, the sheath gas flow rate of 600 L · h ^- 1, using first - order full scan and second - order full - scan modes, the mass range was from 50 to 1000. Results： TLC method is simple, rapid, specific, which can be used for rapid screening; HPLC - PDA method can accurately detect the content of acetaminophen, by which there were 3 batches detected in five batches of samples and 2 batches not detected;UPLC - MS method for struc-tural confirmation is highly characteristic and accurate. Conclusion： The method is confirmatory, highly sensitive and applicable to detect illegal added paracetamol in Chinese patent medicines.