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超高效液相色谱串联质谱法快速检测柑橘中的5种链格孢霉毒素
Rapid Determination of Five Alternaria Mycotoxins in Citrus by Ultra-high Performance Liquid ChromatographyTandem Mass Spectrometry
【摘要】 建立了超高效液相色谱-串联质谱法快速检测柑橘中腾毒素、链格孢酚、交链格孢酚单甲醚、交链孢烯和细交链格孢菌酮酸5种链格孢霉毒素的新方法。样品经改进的QuEChERS(快速、简单、廉价、高效、灵活和安全)方法一步完成萃取净化,采用乙腈-甲酸(1.5%)提取,无水MgSO4和NaCl盐析,以ACQUITY UPLC BEH C18柱为分离柱,用乙腈和0.1%甲酸溶液进行梯度洗脱,电喷雾正离子(ESI+)多反应模式监测,超高效液相色谱-串联质谱(UPLC-MS/MS)测定。在本方法条件下,5种链格孢霉毒素在2.0-100μg/L浓度范围内均呈现良好的线性关系(R2>0.9922),检出限在0.11-0.91μg/kg之间。在5.20和100μg/kg加标水平下,5种毒素的回收率在71%-112%之间,相对标准偏差为1.1%-9.9%,能满足柑橘中链格孢霉毒素检测的要求。
【Abstract】 A novel method was developed for the rapid determination of five alternaria mycotoxins,alternariol,alternariol monomethyl ether,altenuene,tentoxin and tenuazonic acid,in citrus using ultra-high performance liquid chromatography-tandem mass spectrometry.The sample was prepared using the modified QuEChERS(quick,easy,cheap,effective,rigged,and safe) method to complete the extraction and cleanup steps in one procedure.In this QuEChERS method,sample was extracted with acetonitrile(1.5% formic acid),then salted out with anhydrous MgSO4 and NaCl,separated on an ACQUITY UPLC BEH C18 with gradient elution by using acetonitrile and 0.1% formic acid aqueous as eluant,and detected by UPLC-MS /MS under negative(ESI+) electrospray ionization and MRM models.Under these conditions,five alternaria mycotoxins made a good linearity in the concentration range of 2.0- 100 μg/L with R2>0.9922,and the limits of detection of the instrument were in the range of 0.11-0.91 μg/kg.Three spiked levels of five altenaria mycotoxins at 5,20 and 100 μg/kg were investigated,and the recoveries ranged from 71% to 112% with the relative standard deviations(RSDs) varying from 1.1% to 9.9%,which met the requirement of mycotoxins determination.
【Key words】 Altenaria mycotoxins; Ultra-high performance liquid chromatography-tandem mass spectrometry; Citrius; QuEChERS method;
- 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2015年12期
- 【分类号】O657.63;TS255.7
- 【被引频次】44
- 【下载频次】809