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目的:建立检测银翘解毒制剂中是否非法添加解热镇痛药对乙酰氨基酚的方法。方法:采用高效液相色谱法。色谱柱为Waters C18(250mm×5.0mm,4.6μm),流动相为甲醇-0.5%冰醋酸溶液(2∶98,V/V),检测波长为249nm,柱温为30℃,流速为1ml/min,进样量为5μl。在此条件下检测了73个厂家205批样品,并在未检出对乙酰氨基酚的样品中添加适量对照品作为阳性参比对照进行检测。结果:对乙酰氨基酚的进样量在0.0507～1.0104μg范围内与其峰面积积分值呈良好的线性关系(r=0.9999);检出限为0.4ng。银翘解毒片、丸、颗粒的平均加样回收率分别为99.9%(RSD=0.7%,n=6)、96.9%(RSD=0.6%,n=6)、97.6%(RSD=0.4%,n=6)。阳性参比对照均检出对乙酰氨基酚,205批样品均未检出。结论:该方法专属性强、灵敏度高、操作方便,可用于检测中成药中是否非法添加对乙酰氨基酚。
OBJECTIVE: To establish a method for detecting acetaminophen in Yin Qiao detoxification preparations illegally adding antipyretic and analgesic drugs. Methods: Using high performance liquid chromatography. The chromatographic column was Waters C18 (250 mm × 5.0 mm, 4.6 μm). The mobile phase was methanol-0.5% glacial acetic acid (2:98 V / V), the detection wavelength was 249 nm, the column temperature was 30 ℃, the flow rate was 1 ml / min, injection volume of 5μl. Under these conditions, 205 batches of samples from 73 factories were tested, and the appropriate reference substance was added to the samples without acetaminophen as the positive reference control. Results: The calibration curve of paracetamol showed a good linear relationship with the peak area (r = 0.9999) in the range of 0.0507-1.0104μg. The detection limit was 0.4ng. The average recoveries of Yinqiao Jiedu tablets, pills and granules were 99.9% (RSD = 0.7%, n = 6), 96.9% (RSD = 0.6%, n = 6) and 97.6% (RSD = 0.4% n = 6). Paracetamol was detected in both positive and negative controls, and none of the 205 batches of samples was detected. Conclusion: The method is highly specific, sensitive and easy to operate. It can be used to detect the presence of acetaminophen illegally added to proprietary Chinese medicines.