摘要
建立婴幼儿辅食果泥中细交链孢菌酮酸、腾毒素、交链孢酚单甲醚、交链孢酚和交链孢烯5种链格孢霉毒素的QuEChERS-超高效液相色谱-串联质谱分析方法。待测样品经乙腈-水-甲酸混合液(79∶20∶1,V/V/V)提取,4 g无水硫酸镁、0.5 g无水乙酸钠和0.5 g氯化钠脱水盐析,100 mg C18净化,经Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm)液相色谱柱分离,以5 mmol·L^(-1)的乙酸铵水溶液和甲醇作为流动相梯度洗脱,在电喷雾离子源电离,多反应监测模式条件下进行测定,基质外标法定量。该方法在0.1~200μg·L^(-1)范围内线性关系良好,决定系数(R^(2))均大于0.998,检测限和定量限分别为0.1μg·kg^(-1)和0.3μg·kg^(-1)。不同加标水平的平均回收率为73.8%~118.0%,相对标准偏差为2.3%~8.5%。结果表明,该方法高效、准确、灵敏,适用于婴幼儿辅食果泥中5种链格孢霉毒素确证检测。
A QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of five Alternaria toxins including tenuazonic acid,tentoxin,aletrnariol monomethyl ether,alternariol and altenuene in fruit puree for infants was established.A fruit puree sample was extracted with a mixture solution of acetonitrile∶water∶formic acid(79∶20∶1,V/V/V),followed by a salting-out extraction using 0.5 g anhydrous CH_(3)COONa and 0.5 g NaCl coupled with a dehydration step with the addition of 4 g anhydrous MgSO_(4),and a purification step with 100 mg C18.An ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm)was used for chromatographic separation.The mobile phase consisted of 5 mmol·L^(-1) ammonium acetate aqueous solution and methanol and a gradient elution program was applied.The measurement was carried out under the condition of multiple response monitoring mode and electrospray ion source.The matrix-matched external standard was used for quantitative analysis.The linearity of the method was in the range of 0.1-200μg·L^(-1),with the determination coefficients(R^(2))greater than 0.998.The limits of detection and quantification were 0.1μg·kg^(-1) and 0.3μg·kg^(-1),respectively.The average recoveries were in the range of 73.8%to 118.0%with the relative standard deviations of 2.3%to 8.5%.The results demonstrated that the developed method was efficient,accurate,sensitive,and suitable for the quantitative determination of five Alternaria toxins in fruit puree for infants.
作者
邓涛
杨华
肖英平
汪雯
吕文涛
王小骊
吴振
吉小凤
DENG Tao;YANG Hua;XIAO Yingping;WANG Wen;LYU Wentao;WANG Xiaoli;WU Zhen;JI Xiaofeng(College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo 315000,Zhejiang,China;Institute of Agro-Product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)
出处
《浙江农业学报》
CSCD
北大核心
2022年第12期2728-2739,共12页
Acta Agriculturae Zhejiangensis
基金
国家重点研发计划政府间合作项目(2019YFE0103900)。