摘要
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.
出处
《中国食品卫生杂志》
北大核心
2013年第3期249-253,共5页
Chinese Journal of Food Hygiene
基金
北京农业职业学院院级课题(NO.XY-YF-12-18)