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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 UPLCBEHC18(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 supplementary test to check the addition of acetaminophen in Tianma Capsule. Methods: The rapid screening was carried out by TLC method. The HPLC-PDA method was used for quantitative analysis. The chromatographic column was Polaris C18 (4.6 mm × 250 mm, 5 μm) with the mobile phase of methanol-0.6% acetic acid (10:90) 1.0 mL · min-1. The detection wavelength was 243 nm and the column temperature was 30 ℃. Rapid identification was performed by IR method. The structure was confirmed by UPLC-MS. The chromatographic column was Acquity UPLCBEHC18 (50 mm × 2.1 mm × 1.7 μm). The mobile phase consisted of 0.1% formic acid-acetonitrile (5:95) at a flow rate of 0.4 mL.min-1. The mass spectrometry conditions were positive ion detection, electrospray ionization source (ESI), source voltage of 3.1 kV, capillary temperature of 400 ℃, cone voltage of 30 V and sheath gas flow rate of 600 Lh-1. Level full scan mode, the quality of the range of 50 to 1000. Results: The TLC method was simple, rapid and specific, and could be used as a rapid screening method for illegitimate addition. HPLC-PDA method could accurately detect the content of acetaminophen added. Three batches of 5 batches of samples were detected, Not detected; UPLC-MS method to confirm the structure, characteristic, high accuracy. Conclusion: This method is suitable for the determination of paracetamol in Chinese patent medicines illegally added, with strong corroboration and high sensitivity.