阴离子交换固相萃取-超高效液相色谱-串联质谱法检测猪肌肉中13种喹诺酮类药物

Determination of 13 quinolone antibiotic residues in swine muscle by anion exchange solid-phase extraction-ultra high performance liquid chromatography-triple quadrupole mass spectrometer

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 A method was developed for the simultaneous determination of 13 quinolone （QNs） antibiobtics in Swine muscle by ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. Methods The analytes were extracted from the sample using phosphate solution with ultrasonic bath and purified by anion exchange solid- phase extraction （SPE） cartridge. The residue was dried under nitrogen and redissolved for UPLC-MS/MS. The interference of matrix was reduced by the matrix-matched calibration standards curve. Results The linearity arrange was from 5μg/kg to 100 μg/kg for 13 QNs with correlation coefficients from 0. 991 0 -0. 999 2. The limit of quantification was 0. 255 -3. 322 μg/kg. The recoveries were 69.18% - 104.45% with relative standard deviations of 0. 21% - 10. 98%. Conclusion The analytical method is simple, accurate, sensitive and suitable for the determination of 13 quinolone （QNs） antibiobtics in swine muscle.