在线净化-高分辨质谱测定动物源性食品中的糖肽类抗生素
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摘要
为了检测动物源性食品中糖肽类抗生素万古霉素和去甲万古霉素的残留量,采用在线净化与Q Orbitrap高分辨质谱联用技术,在优化的实验条件下,样品提取液经在线净化柱C18-XL净化,资生堂CAPCELL PAK色谱柱分离,以乙腈-0.1%甲酸溶液为流动相,进行梯度洗脱,在Full Scan/dd MS2正离子扫描模式下进行检测.结果表明,万古霉素、去甲万古霉素在0.1—50 ng·m L~(-1)质量浓度范围内呈良好线性关系(r>0.998),定量限为0.3μg·kg~(-1).对空白样品分别加标0.3、1.5、3μg·kg~(-1),回收率为80.2%—93.2%,相对标准偏差RSD为2.8%—9.4%.
In order to detect the residues of vancomycin and norvancomycin which are glycopeptide antibioticsins in animal derived foods,a fast analysis method was implemented on a chromatographic system containing online solidphase extraction( SPE) device that combined with high resolution mass spectrometer( HRMS). Under optimized experimental conditions,the analytes added to blank samples were extracted with appropriate solvent,then purified and enriched on a C18-XL column,whereafter eluted from the purification column onto the analytical columnn( Shiseido CAPCELL PAK ADME column) for chromatographic separation using a gradient elution of 0.1% formic acid water solution and acetonitrile solution. Analytes were detected by Q Orbitrap in positive ion mode with Full Scan/dd MS2. The results showed that the limit of quantitation( LOQ) for each analyte was 0.3 μg·kg-1. In the range of 0.1—50 ng·m L~(-1),the linearity for each analyte was satisfactory and the value of correlation coecient( r) was more than 0.998. The average recoveries spiked at 0.3,1.5 and 3 μg·kg-1were ranged from 80.2% to 93.2%,with the relative standard deviations( RSDs) of 2.8%—9.4%.
In order to detect the residues of vancomycin and norvancomycin which are glycopeptide antibioticsins in animal derived foods,a fast analysis method was implemented on a chromatographic system containing online solidphase extraction( SPE) device that combined with high resolution mass spectrometer( HRMS). Under optimized experimental conditions,the analytes added to blank samples were extracted with appropriate solvent,then purified and enriched on a C18-XL column,whereafter eluted from the purification column onto the analytical columnn( Shiseido CAPCELL PAK ADME column) for chromatographic separation using a gradient elution of 0.1% formic acid water solution and acetonitrile solution. Analytes were detected by Q Orbitrap in positive ion mode with Full Scan/dd MS2. The results showed that the limit of quantitation( LOQ) for each analyte was 0.3 μg·kg-1. In the range of 0.1—50 ng·m L~(-1),the linearity for each analyte was satisfactory and the value of correlation coecient( r) was more than 0.998. The average recoveries spiked at 0.3,1.5 and 3 μg·kg-1were ranged from 80.2% to 93.2%,with the relative standard deviations( RSDs) of 2.8%—9.4%.
引文
[1]彭斯维,陈永刚,邹吉利.酶放大免疫法测定去甲万古霉素的血药浓度[J].广东药学院学报,2014,30(5):553-558.PENG S W,CHEN Y G,ZOU J L. The enzyme amplification immunoassay was used to determine the blood concentration of methycin[J].Journal of Guangdong Academy of Pharmacy,2014,30(5):553-558.