摘要
探讨固相萃取方法,超高效液相色谱串联质谱仪(UPLC-MS/MS)测定麦芯粉中4种交链孢毒素。样品经0.05 mol/L Na H2PO4(pH 3.0)-乙腈-甲醇超声提取(450+450+100,V/V),上清液过HLB固相萃取柱净化,以1.0 mmol/L氨水溶液(pH 8.3)-甲醇为流动相,经Waters CORTECS C18(4.6×100 mm,2.7μm)柱分离梯度洗脱,采用电喷雾负离子(ESI-)、多反应监测(MRM)模式检测;以基质加标工作曲线定量。细交链孢菌酮酸(TeA)、交链孢酚(AOH)在2.0μg/L^100μg/L浓度范围内,腾毒素(TEN)、交链孢酚单甲醚(AME)在0.2μg/L^10.0μg/L浓度范围内线性关系良好,相关系数(R2)均大于0.998。回收率为76.3%~107.5%,TeA、AOH检出限和定量限分别为1.0μg/kg和3.0μg/kg、TEN、AME检出限和定量限分别为0.1μg/kg和0.3μg/kg。该方法灵敏度高,简便,准确。适于测定麦芯粉中的交链孢毒素。
A sensitive and rapid method based on solid phase extraction （SPE） and ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） was developed for the determination of four individual Alternaria toxins in the wheat flour. The samples were extracted with the mixture of 0.05 mol/L NaH2PO4 （pH3.0）-acetonitrile-methanol （450＋450＋100, V/V） by ultrasound, and then purified by HLB solid-phase exlraction column. The separation used Waters CORTECS C18 （4.6x100 mm, 2.7 μm） column gradient elution with 1.0 mmol/L ammonia solution （pH 8.3） and methanol as the mobile phase. The electrospray negative ion （ESI＇） and multiple reaction monitoring mode （MRM） pattern were used to detect and the matrix additive standard was used toquantify the Alternaria Toxins. The tenuazonic acid（TeA） and altemariol （AOH） in concentration range of 2.0--100 μg/L, as well as tentoxin （TEN） and altemariol methyl ether （AME） in concentration range of 0.2-10.0 μg/L, had a good linear relationship with the correlation coefficient （R2） of 〉 0.998. The average recovery was 76.3%-107.5%. The detection limit and the quantitative limit of TeA, AOH, TeA and AME were 1.0 μg/kg and 3.0 μg/kg, respectively. The detection limit and the quantitative limit were 0.1 μg/kg and 0.3 μg/kg, respectively. Therefore, the method is suitable for the determination of Alternaria toxins in flour.
出处
《现代食品科技》
EI
CAS
北大核心
2017年第11期251-256,共6页
Modern Food Science and Technology
基金
江苏省医学重点学科-流行病学资助项目(ZDXKA2016008)
关键词
交链孢毒素
固相萃取
超高效液相色谱串联质谱
Alternaria toxins
solid-phase extraction
ultra-high performance liquid chromatography-tandem mass spectrometry
