渔用配合饲料中左旋肉碱含量的测定  

Determination of L-carnitine in fish formula feed by hydrophilic liquid chromatography-tandem mass spectrometry

作　　者：马瑞欣 李同庆 张志华 MA Rui-xin;LI Tong-qing;ZHANG Zhi-hua(Hebei Fisheries Technology Extension General Station,Hebei Monitoring and Testing Station for Aquatic Products Quality.Shijiazhuang 050035,China)

机构地区：[1]河北省水产技术推广总站,河北省水产品质量检验监测站,河北石家庄050035

出　　处：《河北渔业》2020年第5期38-41,61,共5页

摘　　要：建立了亲水作用色谱-串联质谱法(HILIC-MS/MS)检测渔用配合饲料中左旋肉碱含量的方法。样品用超纯水超声提取,提取液稀释后经HILIC色谱柱分离,以乙腈和乙酸铵(含0.15%甲酸)溶液为流动相梯度洗脱,三重四级杆串联质谱多反应监测(MRM)方式扫描,外标法定量。结果表明,左旋肉碱在0.2~100 ng/mL范围线性良好(r>0.999);检出限0.5μg/kg,定量限1.5μg/kg。在20、50和100 mg/kg添加水平下,回收率为75.2%~111%,相对标准偏差RSD为3.4%~9.9%(n=6)。该方法前处理简单、快速,定性定量准确,适合于渔用配合饲料中左旋肉碱的准确定性定量。An analytical method was developed for the determination of L-carnitine in fish formula feed by using hydrophilic interaction chromatography-tandem mass spectrometry(HILIC-MS/MS). The samples were extracted with ultrapure water by ultrasonic. The separation of L-carnitine was carried out on a Hypersil GOLD HILIC column using ammonium acetate(0.15% formic acid) and acetonitrile as mobile phases. The quantification analysis of the target compoundwas performed under multiple reaction monitoring(MRM) mode by external standard method. A good linear relationship was obtained between the peak area and concentration of L-carnitine in the range of 0.2~100 ng/mL with the correlation coefficient more than 0.999. The limit of detection(LOD)was 0.5 μg/kg and the limit of quantification(LOQ) was 1.5 μg/kg. At spiked levels of 20,50 and 100 mg/kg, the recoveries ranged from 75.2% to 111%, and the relative standard deviation ranged from 3.4% to 9.9%.The sample preparation was simple and rapid, and the results were accurate. The developed method is suitable for the determination of L-carnitine in in fish formula feed.

关 键 词：亲水作用色谱-串联质谱 左旋肉碱 渔用配合饲料 

分 类 号：S963[农业科学—水产养殖]