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液质联用法快速测定饲料中维吉尼亚霉素含量

ISSN号：1005-6521
期刊名称：《食品研究与开发》
时间：0
分类：TQ460.4[化学工程—制药化工]
作者机构：[1]中国海洋大学化学化工学院,山东青岛266100, [2]山东出入境检验检疫局检验检疫技术中心,山东青岛266002
相关基金：国家自然科学基金重点项目（NO.41030858）;国家自然科学基金创新研究群体项目（NO.41221004）

作者：曹文卿[1,2], 吴振兴[2], 静平[2], 杨桂朋[1], 林黎明[2]

关键词：维吉尼亚霉素M_1和S_1, 高效液相色谱-质谱/质谱, 乙腈提取, 冷冻脱脂, 盐析净化, 饲料, 快速测定, HPLC-MS/MS, acetonitrile extraction, freezing de-fatted, salting-out effect, feeds, rapid method

中文摘要：

建立了饲料中快速测定维吉尼亚霉素M_1和S_1残留量的高效液相色谱-质谱/质谱（HPLC-MS/MS）方法。样品采用乙腈提取,经冷冻脱脂和饱和氯化钠溶液盐析净化,用甲醇-甲酸铵溶液定容,经SDB-C8色谱柱分离后,采用多反应监测（MRM）正离子模式检测,监测离子对分别为M1：m/z 526.3/355.1和526.3/337.2;S1：824.5/290.1和824.5/205.1。其中526.3/355.1和824.5/205.1分别用于M_1和S_1的外标法定量。维吉尼亚霉素M_1和S_1在1.0μg/kg~1 000.0μg/kg范围内线性关系良好,相关系数为0.998 7~0.999 5,添加饲料中添加水平为2.0、5.0、10.0μg/kg时,回收率在81.0%~105.0%之间,相对标准偏差（RSD）均小于4.0%（n=6）,最低检出限和定量限分别为1.0μg/kg和2.0μg/kg。实验结果表明,该方法准确度高,省时,操作简单,成本低,重现性好,结果可靠,实用性强。

英文摘要：

A high performance liquid chromatography-tandem mass spectrometric （HPLC-MS/MS）method was developed for the determination of virginiamycin （VGM） M1 and S1 residues in feeds. The samples were extracted with acetonitrile, purified by freezing de-fatted and salting-out effect of saturated sodium chloride solution and redissolved in methanol-ammonium formate solution. The extracts were separated with XDB-C8 LC column using a binary eluent under gradient elution and determined by tandem mass spectrometry under positive electrospray ionization mode with multiple reaction monitoring （MRM） mode. m/z M1：526.3/355.1 and 526.3/337.2,S1：824.5/290.1 and 824.5/205.1 were selected as precursor-product ion pairs, in which 526.3/355.1 and 824.5/205.1 were used for external standard quantization. Under the optimal conditions , the calibration curve was linear over the concentration of VGM in the range of 1.0 μg/kg-1 000.0 μg/kg with correlation coefficient between 0.998 7-0.999 5. The quantitation limit of 2.0μg/kg and the detection limit was 1.0μg/kg. The average fortified recoveries of VGM from feeds at 3 spiked levels of 2.0 , 5.0 and 10μg/kg ranged from 81.0%to 105.0%with relative standard deviations（RSD）（n=6） less than 4.0%. The method showed good simplicity, sensitivity, stability, accuracy, time saving and low cost, and was suitable for the rapid determination of VGM in feedstuffs.