QuEChERS-超高效液相色谱-串联质谱法同时测定婴幼儿辅食果泥中5种链格孢霉毒素

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, 1.8 μm)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0.1~200 μg·L^-1 范围内线性关系良好,决定系数(R²)均大于0.998,检测限和定量限分别为0.1 μg·kg^-1 和0.3 μg·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。

Simultaneous determination of five Alternaria toxins by QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry in fruit puree for infants

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 CH₃COONa and 0.5 g NaCl coupled with a dehydration step with the addition of 4 g anhydrous MgSO₄, and a purification step with 100 mg C18. An ACQUITY UPLC^® HSS T3 column (2.1 mm×100 mm, 1.8 μm) 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 0.1-200 μg·L^-1, with the determination coefficients (R²) greater than 0.998. The limits of detection and quantification were 0.1 μg·kg^-1 and 0.3 μg·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.