目的: 建立一种快速、准确测定远红外贴中16个非法添加药物(10种非甾体类抗炎药和6种糖皮质激素药)的方法。方法: 样品经冷凝回流后,用高效液相色谱法(HPLC)及高分辨液质联用法(UPLC-HRMS/MS)对非法添加药物进行定性分析,并使用高效液相色谱法(HPLC)进行含量测定。结果: 16个非法添加药物在相应测定范围内线性关系良好,相关系数均大于0.999;在3个浓度加标水平下,回收率为81.1%~112.7%;RSD为0.010%~2.8%;各药物检测下限为0.05~1.5 μg·mL-1;定量下限为0.2~5 μg·mL-1;35批样品中9批次检出双氯芬酸钠成分,含量为0.56~37.11 mg·贴-1。结论: 该方法操作简便,专属性强,灵敏度、准确度高,适用于远红外贴及同类产品中非法添加药物的检测。
Objective: To establish a rapid and accurate method for the identification and determination of 16 drugs illegally added in far infrared stickers. Methods: Samples were refluxed in methanol. High performance liquid chromatography (HPLC) and liquid chromatography tandem high resolution mass spectrometry (LC-HRMS/MS) were used for qualitative analysis of illegally added drugs, and HPLC was used for content determination. Results: The 16 compounds showed good linear relationship within their ranges, and the correlation coefficients(r) were above 0.999. Under three different concentration levels, the recoveris ranged from 81.1% to 112.7% with the RSDs of 0.010% to 2.8% at the three concentration levels. The LODs were in range of 0.05-1.5 μg·mL-1 and the LOQs were in range of 0.2-5 μg·mL-1. Diclofenac sodium was detected in 9 of the 35 samples in range of 0.56-37.11 mg per sticker. Conclusion: The method is simple, specific, highly sensitive and accurate, and can be used for the detection of the 16 drugs illegally added in far infrared stickers and similar products.
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