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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

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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C18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20~1 000 μg/L浓度范围内,交链孢烯、格孢毒素I、腾毒素、AAL Toxin TA1在5~200 μg/L浓度范围内均呈现良好的线性关系,其相关系数R2>0.9991,检出限在0.2~3.0 μg/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.
Rapid Determination of Seven Alternaria Toxins in Feed by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
A novel ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/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 acetonitrile-formic acid(1%)and then purified with solid sorbents.The separation of the seven alternaria toxins was performed in a C18 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(R2>9991)in the concentration range of 20-1 000 μg/L,the other alternaria toxins(altenuene,altertoxin I,AAL Toxin TA1,and tentoxin)showed good linearity(R2>9991)in the concentration range of 5-200 μg/L,and the detection limits were in the range of 0.2-3 μg/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.

FeedAlternariaUltra liquid chromatography-tandem mass spectrometry

刘敏海、张艳、谭婷、郭岚、刘翻、万益群

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南昌大学化学化工学院,江西南昌 330031

江西中医药大学药学院,江西南昌 330004

南昌大学分析测试中心,江西南昌 330031

饲料 链格孢霉 高效液相色谱-串联质谱

江西省自然科学基金江西省市场监督管理局科技项目

20232BAB206157GSJK202009

2024

分析科学学报
武汉大学,北京大学,南京大学

分析科学学报

CSTPCD北大核心
影响因子:0.717
ISSN:1006-6144
年,卷(期):2024.40(5)