超高效液相色谱-串联质谱法快速检测饲料中7种链格孢霉毒素  

Rapid Determination of Seven Alternaria Toxins in Feed by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘敏海 张艳 谭婷 郭岚 刘翻 万益群[1,2] LIU Minhai;ZHANG Yan;TAN Ting;GUO Lan;LIU Fan;WAN Yiqun(School of Chemistry and Chemical engineering,Nanchang University,Nanchang 330031;Center of Analysis and Testing,Nanchang University,Nanchang 330031;School of Pharmacy,Jiangxi University of Chinese Medicine,Nanchang 330004)

机构地区：[1]南昌大学化学化工学院,江西南昌330031 [2]南昌大学分析测试中心,江西南昌330031 [3]江西中医药大学药学院,江西南昌330004

出　　处：《分析科学学报》2024年第5期524-532,共9页Journal of Analytical Science

基　　金：江西省自然科学基金(20232BAB206157);江西省市场监督管理局科技项目(GSJK202009).

摘　　要：建立了一种新型超高效液相色谱-串联质谱分析方法快速检测饲料中细交链格孢菌酮酸、交链孢酚、交链格孢酚单甲醚、交链孢烯、格孢毒素I、AAL Toxin TA1和腾毒素共7种链格孢霉毒素。使用改进的QuEChERS方法用于饲料样品中目标物的提取和净化,目标物经1%甲酸-乙腈提取后用固体吸附剂进行净化,使用C_(18)柱对7种链格孢霉毒素进行分离,电喷雾正离子模式进行监测。结果显示,细交链格孢菌酮酸、交链孢酚、交链格孢酚单甲醚在20~1000μg/L浓度范围内,交链孢烯、格孢毒素I、腾毒素、AAL Toxin TA1在5~200μg/L浓度范围内均呈现良好的线性关系,其相关系数R^(2)>0.9991,检出限在0.2~3.0μg/L之间。7种链格孢霉毒素的样品加标回收率在73.8%~117.4%之间,相对标准偏差(n=6)为1.5%~9.9%。本方法检测饲料中的链格孢霉毒素具有较高的准确度和灵敏度,可以用于饲料中链格孢霉毒素的检测,对于饲料安全监控具有实际意义。A novel ultra performance liquid chromatographytandem mass spectrometry(UPLCMS/MS)method was developed for rapid determination of seven alternaria toxins(tenuazonic acid,alternariol,alternariol monomethyl ether,altenuene,altertoxin I,AAL Toxin TA1,and tentoxin)in feed samples.A modified QuEChERS method was used for the extraction and purification of the targets from the feed samples.The seven alternaria toxins were firstly extracted by acetonitrileformic acid(1%)and then purified with solid sorbents.The separation of the seven alternaria toxins was performed in a C_(18) column.Electrospray positive ionization mode was chosen for monitoring.The results showed that three alternaria toxins(tenuazonic acid,alternariol,alternariol monomethyl ether)showed good linearity(R^(2)>9991)in the concentration range of 20-1000μg/L,the other alternaria toxins(altenuene,altertoxin I,AAL Toxin TA1,and tentoxin)showed good linearity(R^(2)>9991)in the concentration range of 5-200μg/L,and the detection limits were in the range of 0.2-3μg/L.The spiked recoveries of seven toxins were in the range of 73.8%-117.4% with RSD(n=6)of 1.5%-9.9%.All above results showed that the method was accurate and sensitive and could be used for the detection of alternaria toxins in feeds,which was of practical significance for the monitoring of feed safety.

关 键 词：饲料 链格孢霉 高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]