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建立了固相萃取-高效液相色谱-二极管阵列(SPE-HPLC-DAD)法同时测定中成药及保健品中可能违禁添加的20种非甾体抗炎药(NSAIDs)。样品经甲醇超声提取,以Oasis HLB固相萃取柱净化后检测。采用Waters XBridge Shield RP C18色谱柱;以0.02 mol/L乙酸铵溶液(p H 5.0)和乙腈为流动相,梯度洗脱;检测波长230 nm和280 nm。结果表明,样品经净化后,基质对测定干扰较小,20种NSAIDs均在1~50?g/ml范围内线性关系良好;检测限(LOD)为0.03~0.80 mg/kg。
A total of 20 non-steroidal anti-inflammatory drugs (NSAIDs), which may be banned in proprietary Chinese medicines and nutraceuticals, were simultaneously determined by SPE-HPLC-DAD. The samples were extracted by methanol and purified by Oasis HLB SPE cartridge. A Waters XBridge Shield RP C18 column was used. The mobile phase was eluted with 0.02 mol / L ammonium acetate solution (p H 5.0) and acetonitrile. The detection wavelength was 230 nm and 280 nm. The results showed that the matrix had little interference with the assay after purification. The linearity of the 20 NSAIDs ranged from 1 to 50 μg / ml. The limit of detection (LOD) was 0.03-0.80 mg / kg.