CAJ | 학술논문

建立了牛奶中氯霉素、甲砜霉素和氟甲砜霉素多残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取，以MGⅢ-C18色谱柱（2.1×150 mm，5μm）分离，流动相为10 mmol/L乙酸铵水溶液和甲醇（梯度洗脱），流速0.25 mL/min。采用多反应监测负离子模式，可以同时对牛奶中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量测定。方法的检出限为0.1μg/kg～0.3μg/kg。在0.3、3.0、10.0μg/kg 3个加标水平下，加标回收率为80.7%~93.6%，相对标准偏差为3.85%~9.35%。
건립료우내중록매소、갑풍매소화불갑풍매소다잔류적고효액상색보-천련사겁간질보련용측정방법。양품경감성을정초성제취，이MGⅢ-C18색보주（2.1×150 mm，5μm）분리，류동상위10 mmol/L을산안수용액화갑순（제도세탈），류속0.25 mL/min。채용다반응감측부리자모식，가이동시대우내중적록매소、갑풍매소화불갑풍매소진행정성화정량측정。방법적검출한위0.1μg/kg～0.3μg/kg。재0.3、3.0、10.0μg/kg 3개가표수평하，가표회수솔위80.7%~93.6%，상대표준편차위3.85%~9.35%。
A quick confirmative method was developed for determining the residues of chloramphenicol , thiamphenicol and florfenicol in milk by LC-MS/MS. The sample was ultrasonic extracted with alkaline acetonitrile, the HPLC separation was carried out on a MGⅢ-C18 column (2.1×150 mm, 5μm),the mobile phase were 10 mmol/L ammonium acetate solution and methanol with gradient elution , the flow was 0.25 mL/min.The detection of chloramphenicol , thiamphenicol and florfenicol were carried out in the negative multi-reaction monitoring (MRM)mode. Under the optimal conditions, good linear relationship were obtained in the range of 0.1 μg/kg-50.0 μg/kg for chloramphenicol , thiamphenicol and florfenicol.The limit of detection were in the range of 0.1μg/kg-0.3μg/kg. The recoveries at three spiked levels of 0.3、3.0、10.0μg/kg were between 80.7%and 93.6%, and RSDs value were between 3.85%and 9.35%.