食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
4期
1167-1173
,共7页
刘佳%梁桂荣%李少晖%谢云峰%任丹丹%杨永坛
劉佳%樑桂榮%李少暉%謝雲峰%任丹丹%楊永罈
류가%량계영%리소휘%사운봉%임단단%양영단
β2-受体激动剂%液相色谱-串联质谱法%饲料%残留
β2-受體激動劑%液相色譜-串聯質譜法%飼料%殘留
β2-수체격동제%액상색보-천련질보법%사료%잔류
β2-Agonist%high performance liquid chromatography-tandem mass spectrometry%feed%residues
目的:建立一种饲料中26种β2-受体激动剂兽药残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经盐酸甲醇提取液提取,醋酸铅沉淀蛋白后,过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测。结果本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在20、50和100μg/L添加水平的回收率为71.9%~102.9%,相对标准偏差小于11.8%(n=6),方法定量限为10μg/kg。结论该方法快速、准确、灵敏,适合测定饲料中的β2-受体激动剂类药物残留。
目的:建立一種飼料中26種β2-受體激動劑獸藥殘留的液相色譜-串聯質譜(HPLC-MS/MS)檢測方法。方法樣品經鹽痠甲醇提取液提取,醋痠鉛沉澱蛋白後,過混閤暘離子(MCX)固相萃取柱淨化。採用0.1%甲痠(A)和0.1%甲痠-乙腈(B)作為流動相進行梯度洗脫,質譜(ESI+)採用多離子檢測模式(MRM)對β2-受體激動劑的定量離子和定性離子進行鑑測。結果本方法在15 min內完成26種目標化閤物的分離分析。26種β2-受體激動劑在20、50和100μg/L添加水平的迴收率為71.9%~102.9%,相對標準偏差小于11.8%(n=6),方法定量限為10μg/kg。結論該方法快速、準確、靈敏,適閤測定飼料中的β2-受體激動劑類藥物殘留。
목적:건립일충사료중26충β2-수체격동제수약잔류적액상색보-천련질보(HPLC-MS/MS)검측방법。방법양품경염산갑순제취액제취,작산연침정단백후,과혼합양리자(MCX)고상췌취주정화。채용0.1%갑산(A)화0.1%갑산-을정(B)작위류동상진행제도세탈,질보(ESI+)채용다리자검측모식(MRM)대β2-수체격동제적정량리자화정성리자진행감측。결과본방법재15 min내완성26충목표화합물적분리분석。26충β2-수체격동제재20、50화100μg/L첨가수평적회수솔위71.9%~102.9%,상대표준편차소우11.8%(n=6),방법정량한위10μg/kg。결론해방법쾌속、준학、령민,괄합측정사료중적β2-수체격동제류약물잔류。
Objective To determination of26β2-agonist residues in feed samples by liquid chromatography -tandem mass spectrometric (LC–MS/MS).MethodsFeed samples were extracted with muriatic acid and methanol solution. And then theβ2-agonist residues in the extracts were separated on a reversed phase using a gradient elution program of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile solution (B). Using LC–MS/MS (ESI+) with multiple reactions monitoring (MRM), identification of the major components of the 26 kinds ofβ2-agonist residues was performed based upon the intensities of fragments. ResultsThe recoveries were ranged from 71.9% to 102.9% for the 26 kinds ofβ2-agonist residues with 3 spiked levels of 20, 50 and 100μg/kg. The relative standard deviations (RSDs) were less than 11.8% (n=6), and the limits of quantitation (LOQ) for the 26 kinds ofβ2-agonists were 10μg/kg.ConclusionThe proposed method is fast, accurate and sensitive, which is suitable for detectingβ2-agonist residues in feed samples.