摘要
建立高效液相色谱串联质谱法测定饲料中苯乙醇胺A的分析方法。样品用80%(V∶V)乙腈水溶液提取,经PRiME HLB净化后,采用高效液相色谱串联质谱法测定,外标法定量。以0.1%甲酸水溶液和甲醇作为流动相,用Hypersil GOLD C18色谱柱(1.9μm,2.1 mm×100 mm)进行梯度洗脱,采用电喷雾离子源(ESI^(+))、正离子扫描多反应监测(MRM)模式进行定性和定量分析。结果表明:苯乙醇胺A在5.0~200.0 ng·mL^(-1)的范围内线性关系良好(r=0.9992)。在10.0、20.0、50.0μg·kg^(-1)添加水平下的回收率为82.2%~91.5%,相对标准偏差(n=6)为6.8%~8.5%,检出限(以信噪比>3计)为0.1μg·kg^(-1),定量限(以信噪比>10计)为0.3μg·kg^(-1)。该方法精密度好,灵敏度高,可用于大批量快速准确测定饲料中的苯乙醇胺A,有效提高工作效率。
A analytical method for the determination of phenylethanolamine A in feed by high performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted with 80%(V∶V)acetonitrile aqueous solution.After purified by PRiME HLB,the samples were determined by high performance liquid chromatography-tandem mass spectrometry and quantified by external standard method.Then,the gradient elution was performed through Hypersil GOLD C18 chromatographic column(1.9μm,2.1 mm×100 mm)by using 0.1%formic acid aqueous solution and methanol as the mobile phase.And the qualitative and quantitative analysis was carried out by using the modes of electrospray ionization(ESI^(+))and positive-ion scanning multiple reaction monitoring(MRM).The results showed that phenylethanolamine A had a good linear relationship in the range of 5.0~200.0 ng·mL^(-1)(r=0.9992).The recoveries were 82.2%to 91.5%at the supplemented levels of 10.0,20.0 and 50.0μg·kg^(-1),the relative standard deviations(n=6)were 6.8%to 8.5%,the limits of detection(the SNR being greater than 3)were 0.1μg·kg^(-1),and the limits of quantification(the SNR being greater than 10)were 0.3μg·kg^(-1).The method had good precision and high sensitivity,and could be used for the rapid and accurate determination of phenylethanolamine A in large quantities,which would effectively improve the work efficiency.
作者
陈其煌
CHEN Qi-huang(Xiamen Inspection and Test Center of Agricultural Products Quality and Safety, Xiamen, Fujian 361009, China)
出处
《福建农业科技》
CAS
2021年第2期24-31,共8页
Fujian Agricultural Science and Technology
关键词
PRiME
HLB
高效液相色谱串联质谱法
苯乙醇胺A
饲料
PRiME HLB
High performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)
Phenylethanolamine A
Feed
作者简介
陈其煌,男,1970年生,高级农艺师,主要从事农产品质量与安全研究。
