CAJ | 학술논문

建立了一种超高效液相色谱-串联质谱（ UPLC-MS/MS）测定多种基质（鸡肉、鱼肉、鸡肝、鸡蛋和牛奶）中三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶的分析方法。样品用甲酸-乙腈（1：9，v/v）溶液提取，正己烷除脂净化，Acquity UPLC BEH C18柱（50 mm×2.1 mm，1.7μm）分离，以甲醇和5 mmol/L 醋酸铵（含0.1％（v/v）甲酸）作为流动相进行梯度洗脱，电喷雾正离子（ ESI＋）模式电离，多反应监测（ MRM）模式检测。考察了3种提取溶液的提取效率，优化了净化条件和浓缩条件，并对流动相、柱温和固相萃取柱进行了优化。结果表明：三甲氧苄氨嘧啶、二甲氧苄胺嘧啶和二甲氧甲基苄胺嘧啶在1.25~30.0μg/L范围内线性关系良好（ r≥0.99）。方法的定量限（S/N=10）为5.0μg/kg，在5.0、10.0、20.0μg/kg 的添加浓度的回收率为61.2％~108.5％，相对标准偏差（ RSD，n=6）为1.1％~9.8％。该方法快速、灵敏、准确，适合于多种基质中磺胺增效剂的测定。
건립료일충초고효액상색보-천련질보（ UPLC-MS/MS）측정다충기질（계육、어육、계간、계단화우내）중삼갑양변안밀정、이갑양변알밀정화이갑양갑기변알밀정적분석방법。양품용갑산-을정（1：9，v/v）용액제취，정기완제지정화，Acquity UPLC BEH C18주（50 mm×2.1 mm，1.7μm）분리，이갑순화5 mmol/L 작산안（함0.1％（v/v）갑산）작위류동상진행제도세탈，전분무정리자（ ESI＋）모식전리，다반응감측（ MRM）모식검측。고찰료3충제취용액적제취효솔，우화료정화조건화농축조건，병대류동상、주온화고상췌취주진행료우화。결과표명：삼갑양변안밀정、이갑양변알밀정화이갑양갑기변알밀정재1.25~30.0μg/L범위내선성관계량호（ r≥0.99）。방법적정량한（S/N=10）위5.0μg/kg，재5.0、10.0、20.0μg/kg 적첨가농도적회수솔위61.2％~108.5％，상대표준편차（ RSD，n=6）위1.1％~9.8％。해방법쾌속、령민、준학，괄합우다충기질중광알증효제적측정。
A method for the determination of sulfonamide potentiators,trimethoprim( TMP), diaveridine(DVD)and ormetoprin(OMP),in different animal origin food matrices(including chicken muscle,fish muscle,chicken liver,egg and milk)has been developed by ultra perform-ance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS). The sample was extrac-ted by formic acid-acetonitrile(1:9,v/v),cleaned-up by hexane,separated on an Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7 μm)with gradient elution. The determination was car-ried out with electrospray ion source under the positive mode and multiple reaction monitoring ( MRM)mode. The extraction recoveries of three extraction solvents were observed. The purifica-tion condition and concentration condition were optimized. In addition,the mobile phase,col-umn temperature and solid phase extraction column were studied. The calibration curves showed a good linearity in the range of 1. 25-30. 0 μg/L,and the correlation coefficients( r)were higher than 0. 99. The limits of quantification( LOQ,S/N=10)of the three potentiators were 5. 0 μg/kg. At the spiked levels of 5. 0,10. 0 and 20. 0 μg/kg,the recoveries of the three potentiators were ranged from 61. 2% to 108. 5%,and the relative standard deviations( RSD,n=6)ranged from 1. 1% to 9. 8%. The results indicate that the method is simple,rapid,sensitive and suitable for the qualitative and quantitative analysis of the three potentiators in multiple matrices.