CAJ | 학술논문

为建立检测鸡蛋中黏杆菌素A、黏杆菌素B、多黏菌素B3种黏菌素类抗生素的高效液相色谱三重四级杆串联质谱（HPLC/MS QQQ）的方法，对试验过程中的色谱条件、质谱条件、样品前处理方法进行优化。优化的检测方法为鸡蛋样品用5％的高氯酸提取，经乙醚液液萃取后，再用Strata X小柱净化，最后用2g/L的甲酸溶液（A相）和0.1％的甲酸乙腈（B相）溶液作为流动相进行梯度洗脱，应用电喷雾离子源的多反应监测模式（M RM ）对3种物质进行定性和定量分析。结果显示，3种黏菌素类抗生素添加水平在25～200 mg/kg的回收率为75.6％～106.9％，相对标准偏差小于20％，方法检出限为0.11～0.26 mg/kg。建立的鸡蛋中黏菌素残留的检测方法前处理简单易行，便于操作，精密度高，可以满足对鸡蛋中黏菌素类抗生素快速、准确的检测要求，适合大量样品的准确定性和定量分析。
위건립검측계단중점간균소A、점간균소B、다점균소B3충점균소류항생소적고효액상색보삼중사급간천련질보（HPLC/MS QQQ）적방법，대시험과정중적색보조건、질보조건、양품전처리방법진행우화。우화적검측방법위계단양품용5％적고록산제취，경을미액액췌취후，재용Strata X소주정화，최후용2g/L적갑산용액（A상）화0.1％적갑산을정（B상）용액작위류동상진행제도세탈，응용전분무리자원적다반응감측모식（M RM ）대3충물질진행정성화정량분석。결과현시，3충점균소류항생소첨가수평재25～200 mg/kg적회수솔위75.6％～106.9％，상대표준편차소우20％，방법검출한위0.11～0.26 mg/kg。건립적계단중점균소잔류적검측방법전처리간단역행，편우조작，정밀도고，가이만족대계단중점균소류항생소쾌속、준학적검측요구，괄합대량양품적준학정성화정량분석。
To develop a sensitive liquid chromatography tandem mass spectrometric(LC-MS/MS) method for colistin A ,colistin B and polymyxin B inbovine egg samples ,chromatographic condi-tion ,spectrometric condition and the fortreatment of samples were optimized .Egg samples were extracted with 5% Perchloric acid ,and deproteinized with aether ,and purified with Strata-X .The three colistin antibiotics in the extract were separated on a reversed phase using a gradient elution program of 2 g/L formic acid solution (A) and 0 .1% formic acid aqueous solution (B) .Using LC-MS/MS(ESI) with multiple reaction monitoring (MRM ) ,identification of the major components of the three kinds of colistin antibiotics was performed based upon the intensities of mass frag-ments from the respective doubly or triply charged precursor ions .The recoveries were 75 .6% -106 .9% for the three colistins at spiked levels of 25-200 μg/kg ,and the relative standard devia-tion was less than 20% .The limit of detection for the three colistins antibiotics was 0 .11-0 .26μg/kg .The method is suitable for quantitative and qualitative analysis of colistin antibiotics in a sufficient number of samples with simplicity ,sensitivity and repeatability ,and which could meet the request of colistin antibiotic residue testing at home and abroad .