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目的建立猪肌肉中喹诺酮类(QNs)药物液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)检测方法。方法样品经磷酸盐溶液超声提取碱化后,采用阴离子交换固相萃取(SPE)柱净化提取液,并对目标物质进行富集,用UPLC-MS/MS检测猪肌肉中喹诺酮类药物含量。试验通过空白基质净化液添加标准品,建立校正标准曲线,降低基质对离子化的干扰。结果 13种喹诺酮类药品在5~100μg/kg的线性范围内均具有良好的线性关系,相关系数在0.991 0~0.999 2之间,定量限(LOQ)为0.255~3.322μg/kg,回收率均在69.18%~104.45%之间,相对标准偏差为0.21%~10.98%。结论该方法简便、快速、灵敏度高,适用于猪肌肉中喹诺酮类药物的检测需求。
Objective To establish a method for the determination of quinolones (QNs) in swine muscle by liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS / MS). Methods The samples were extracted by phosphatase solution and alkalized. The extracts were purified by anion exchange solid phase extraction (SPE), and the target substance was enriched. The contents of quinolones in pork muscle were determined by UPLC-MS / MS. Test blank matrix purifying solution by adding standards to establish a calibration standard curve to reduce the matrix on the ionization interference. Results Thirteen quinolones showed a good linearity in the range of 5-100 μg / kg with a correlation coefficient of 0.991 0 to 0.999 2 and a limit of quantification (LOQ) of 0.255-3.3322 μg / kg Between 69.18% and 104.45%, the relative standard deviation was 0.21% -10.98%. Conclusion The method is simple, rapid, sensitive and suitable for the detection of quinolones in pig muscle.