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
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马建民 男 讲师 研究方向为兽药残留检测 E-mail:dsy@cau.edu.cn

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北京农业职业学院院级课题(NO.XY-YF-12-18)


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

    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0.9910~0.9992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。

    Abstract:

    A method was developed for the simultaneous determination of 13quinolone (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 100μg/kg for 13QNs with correlation coefficients from 0.9910-0.9992. The limit of quantification was 0.255-3.322μg/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 13quinolone (QNs) antibiobtics in swine muscle.

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马建民,夏曦,李晓薇,丁双阳.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[J].中国食品卫生杂志,2013,25(3):249-253.

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  • 收稿日期:2013-04-02
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  • 在线发布日期: 2013-06-19
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