摘要
本研究通过乙酸钠-乙酸缓冲液提取,经过夜酶解及SCX净化柱净化,高效液相色谱-串联质谱法测定,建立了中华绒螯蟹中β-受体激动剂西马特罗残留量的检测方法,内标法定量。实验结果表明,西马特罗在0.4980~199.2000 ng·mL^(-1)呈现良好的线性关系,线性相关系数大于0.99,方法测定低限为0.5μg·kg^(-1),在1倍、2倍、10倍方法测定低限3个加标水平下进行了方法学考察,中华绒螯蟹基质中西马特罗的平均回收率为87.06%~94.10%,相对标准偏差(n=6)≤8.03%,满足检验检测分析要求,方法具有高灵敏度,高选择性及前处理简便的特点。利用本研究构建的方法对57批次市售中华绒螯蟹实际样品进行检测分析,检出3批次阳性样本,含量范围为1.70~2.86μg·kg^(-1),表明市场中中华绒螯蟹有违规使用西马特罗禁用药物的风险,需要加以关注。
In this study,a HPLC-MS/MS method for the determination ofβ-agonist Cimaterol residues in Chinese mitten crab was developed.By extraction of sodium acetate buffer,digestion withβ-glucuronidase/aryl sulfatase enzyme overnight,and purification with SCX column,the Cimaterol residues was measured by HPLC-MS/MS instrument,and quantified by internal standard method.The results showed that a good linear relationship was found in the range of 0.4980~199.2000 ng·mL^(-1),which linear correlation coefficient was greater than 0.99.This method allowed for the low limit determination of 0.5μg·kg^(-1).Then we investigated the methodology of three spiked levels at one,two and ten times of low limit determination.The average recoveries of Cimaterol from Chinese mitten crab matrix ranged from 87.06%to 94.10%,and the relative standard deviation(n=6)was less than or equal to 8.03%,which met the requirements of detection and analysis.The method was characterized by high sensitivity,high selectivity and simple pretreatment.The method constructed in this study was used to detect and analyze 57 batches of commercial samples of Chinese mitten crab,among them 3 batches of positive samples were detected,with the content ranging from 1.70~2.86μg·kg^(-1),indicating that there is a risk of illegal use of banned drugs Cimaterol in Chinese mitten crab in the market,which needs to be paid attention to.
作者
刘真
王玉梅
LIU Zhen;WANG Yumei(Nanjing Institute for Food and Drug Control,Nanjing 211198,China)
出处
《现代食品》
2022年第4期155-160,174,共7页
Modern Food
