农产品加工·学刊（下）
農產品加工·學刊（下）
농산품가공·학간（하）
Academic Periodical of Farm Products Processing
2014年
7期
54-56
,共3页
海鲈鱼%土霉素%四环素%金霉素%强力霉素%液相色谱串联质谱
海鱸魚%土黴素%四環素%金黴素%彊力黴素%液相色譜串聯質譜
해로어%토매소%사배소%금매소%강력매소%액상색보천련질보
sea perch%oxytetracycline%tetracycline%chlortetracycline%doxycycline%LC/MS/MS
研究建立海鲈鱼中四环素族的液相色谱/串联质谱（LC/MS/MS）方法。海鲈鱼样品经制样，1%高氯酸溶液提取土霉素、四环素、金霉素、强力霉素，固相萃取装置（SPE）净化，氮气吹干后用甲醇复溶。以Welch Materials Ultimate XD-C8色谱分离柱，乙腈-甲醇混合溶液、0.1%甲酸水溶液梯度洗脱，使用电喷雾三重四极杆串联质谱的多重反应监测模式（Multiple Reaction Monitoring，MRM）测定，以校准曲线法进行定量。所建立的液相色谱串联质谱法（LC/MS/MS）对于分析海鲈鱼中土霉素、四环素、金霉素、强力霉素的批内、批间RSD分别为0.12％~0.86％，0.10％~0.37％，回收率为91.7％~95.3％。
研究建立海鱸魚中四環素族的液相色譜/串聯質譜（LC/MS/MS）方法。海鱸魚樣品經製樣，1%高氯痠溶液提取土黴素、四環素、金黴素、彊力黴素，固相萃取裝置（SPE）淨化，氮氣吹榦後用甲醇複溶。以Welch Materials Ultimate XD-C8色譜分離柱，乙腈-甲醇混閤溶液、0.1%甲痠水溶液梯度洗脫，使用電噴霧三重四極桿串聯質譜的多重反應鑑測模式（Multiple Reaction Monitoring，MRM）測定，以校準麯線法進行定量。所建立的液相色譜串聯質譜法（LC/MS/MS）對于分析海鱸魚中土黴素、四環素、金黴素、彊力黴素的批內、批間RSD分彆為0.12％~0.86％，0.10％~0.37％，迴收率為91.7％~95.3％。
연구건립해로어중사배소족적액상색보/천련질보（LC/MS/MS）방법。해로어양품경제양，1%고록산용액제취토매소、사배소、금매소、강력매소，고상췌취장치（SPE）정화，담기취간후용갑순복용。이Welch Materials Ultimate XD-C8색보분리주，을정-갑순혼합용액、0.1%갑산수용액제도세탈，사용전분무삼중사겁간천련질보적다중반응감측모식（Multiple Reaction Monitoring，MRM）측정，이교준곡선법진행정량。소건립적액상색보천련질보법（LC/MS/MS）대우분석해로어중토매소、사배소、금매소、강력매소적비내、비간RSD분별위0.12％~0.86％，0.10％~0.37％，회수솔위91.7％~95.3％。
A measurement method for tetracyclines in sea perch involving LCMS/MS has been developed. The tetracyclines are extracted from sea perch using 1% perchloric acid and cleaned by solid-phase extractions prior to reversed-phase LC/MS/MS determination. Separation is performed on a Welch Materials Ultimate XB-C8 column using gradient elution with acetonitrile - methanol mixed solution and 0.1% formic acid. An agilent tandem mass spectrometer equipped with an electrospmy ionization source operated in multiple reaction monitoring(MRM)mode is utilized,and the results of determination are calculated from the calibration curve. The results of the LC/MS/MS method for the analysis of oxytetracycline,tetracycline,chlortetracycline, doxycycline in sea perch samples are as follows,the within-run RSD ranged from 0.12%to 0.86%,between-run RSD ranged from 0.10%to 0.37%and recoveries ranged between 91.7%~95.3%.
