CAJ | 학술논문

目的：建立鸡肉中4种雄激素,3种孕激素,4种糖皮质激素药物多残留的QuEChERS/超高效液相色谱-串联质谱(ultra pressure liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定方法。方法样品用乙酸乙酯提取,经QuEChERS分散固相萃取净化后,采用phenomenex kinetex色谱柱分离,分别在电喷雾正、负离子模式下以多反应监测(multiple reaction monitoring, MRM)方式检测。正、负离子模式下流动相均为0.1%甲酸水和乙腈梯度洗脱。结果11种药物在相应的浓度范围内线性良好,相关系数均大于0.991,在3个加标水平下的平均回收率为84.4%~94.1%,相对标准偏差(RSD)为7.5%~12.5%,检出限(LOD, S/N≥3)和定量下限(LOQ, S/N≥10)分别为0.37~9.55μg/kg及1.11~28.65μg/kg。结论该方法简便快速、灵敏可靠、经济有效,适用于鸡肉中激素类药物多残留的同时快速测定。
목적：건립계육중4충웅격소,3충잉격소,4충당피질격소약물다잔류적QuEChERS/초고효액상색보-천련질보(ultra pressure liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)동시측정방법。방법양품용을산을지제취,경QuEChERS분산고상췌취정화후,채용phenomenex kinetex색보주분리,분별재전분무정、부리자모식하이다반응감측(multiple reaction monitoring, MRM)방식검측。정、부리자모식하류동상균위0.1%갑산수화을정제도세탈。결과11충약물재상응적농도범위내선성량호,상관계수균대우0.991,재3개가표수평하적평균회수솔위84.4%~94.1%,상대표준편차(RSD)위7.5%~12.5%,검출한(LOD, S/N≥3)화정량하한(LOQ, S/N≥10)분별위0.37~9.55μg/kg급1.11~28.65μg/kg。결론해방법간편쾌속、령민가고、경제유효,괄용우계육중격소류약물다잔류적동시쾌속측정。
Objective A multi-residue testing method was developed for the simultaneous determination of 4 androgens, 3 progesterones and 4 glucocorticoids in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The homogenized sample extracted with ethyl acetate. The separation was performed on a phenomenex kinetex column by gradient elution after puring from dispersive-solid-phase extraction(d-SPE). The analysis of 11 ana-lytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring (MRM). Acetonitrile and water(containing 0.1% formic acid) were used as the mobile phase both in positive and negative. Results The correlation coeficients of calibration curves were over 0.991 in the corresponding concentration range. The average recoveries of the 11 analytes at three spiked concentration levels varied from 84.4%to 94.1%and the relative standard deviations(RSDs) varied from 7.5%to 12.5%. The limits of detection(LOD, S/N≥3) and quantitation(LOQ, S/N≥10) were 0.37~9.55 μg/kg and 1.11~28.65μg/kg, respectively. Conclusion The real sample tests showed that the proposed method was sim-ple, rapid, sensitive, reliable and cost-effective, and it was suitable for the simultaneous determination of hor-mones residues in chicken samples.