天麻胶囊质量标准中补充检验对乙酰氨基酚的方法

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,5 μm),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^® BEH C₁₈(50 mm×2.1 mm×1.7 μm),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 quantitative inspection,the column was Polaris C₁₈ (4.6 mm × 250 mm,5 μm),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 temperature was 30 ℃.IR method was used for rapid identification with UPLC-MS method for the structural confirmation;the column was Acquity UPLC^® BEH C₁₈ (50 mm × 2.1 mm × 1.7 μm),the mobile phase was 0.1% formic 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 structural confirmation is highly characteristic and accurate. Conclusion: The method is confirmatory,highly sensitive and applicable to detect illegal added paracetamol in Chinese patent medicines.