超高压液相色谱法同时检测玉米中的伏马毒素B1、B2、B3
目的 综合比较伏马毒素4种柱前衍生[邻苯二甲醛(OPA)、萘-2,3-二甲醛(NDA)、丹磺酰氯、6-氨基喹啉-N-羟基琥珀酰亚胺氨基甲酸酯(AQC)]效果的优劣, 并选择一种衍生剂用于玉米样品中伏马毒素B1(FB1)、B2(FB2)、B3(FB3)的检测, 建立柱前衍生-超高压液相色谱法同时测定玉米中伏马毒素B1、B2和B3的方法。方法 采用乙腈-水(50∶50, v/v)溶液提取玉米中的伏马毒素B1、B2和B3, 涡旋震荡及离子交换柱净化对玉米样品中的伏马毒素B1、B2和B3进行提取与净化, 经衍生后进行超高压液相色谱-荧光检测器检测。 结果 最终选择OPA衍生作为本研究的衍生方法。3种伏马毒素的线性范围分别为50~1000 ng/mL、25~500 ng/mL、25~500 ng/mL, 相关系数R2均大于0.999; 最低定量限LOQ分别为25.0、14.0、17.0 μg/kg; 3个浓度的加标回收率分别为(75.6?1.6)%~(83.4?2.3)%, (78.9?5.4)%~(90.0?0.7)%, (83.7?8.2)%~(88.6?1.0)%; FB1、FB2和FB3的日间精密度分别为3.62%、3.41%、4.77%。结论 该方法具有预处理简单、检测速度快、灵敏度高的优点, 可满足对玉米中>800 μg/kg伏马毒素含量的检测要求。流动相的改进及梯度洗脱的使用, 提高了检测的灵敏度, 并可被在具有液相色谱仪的实验室应用。
Objective To compare the derivative effects of 4 pre-column derivations [o-phthaldialdehyde (OPA), naphthalene-2,3-dicarboxaldehyde (NDA), Dynsyl chloride, 6-Aminoquinolyl-N-Hydroxysuccinimidyl-carbamate (AQC)] on fumonisins B1, B2 and B3, and select one of which as the derivation in the investigation, so as to establish a method for simultaneous determination of fumonisins B1, B2 and B3 in maize by pre-column ultra pressure liquid chromatography (UPLC). Methods Homogenized samples were extracted by acetonitrile aqueous solution (50：50, v/v) with vortex, and purified by an ion exchange column. And the analytes were detected by UPLC combined by fluorescence detection after derivation. Results The OPA derivatization reagent was selected to be used in the investigation. The linear range was 50~1000 ng/mL for FB1 and 25~500 ng/mL for FB2 and FB3 with linearity coefficients all above 0.999. The LOQs were 25.0, 14.0 and 17.0 μg/kg, respectively. The recoveries were (75.6?1.6)%~(83.4?2.3)%, (78.9?5.4)%~(90.0?0.7)%, and (83.7?8.2)%~ (88.6±1.0)% at 3 spike concentrations, respectively. The RSD of inner-day precision of them ranged from 3.41% to 4.77%. Conclusion The established method is simple, rapid and sensitive, which can successfully meet the minimum level requests of maize from varies countries. The improved mobile phase and the use of gradient program have improved the detection sensitivity, and it can be applied in laboratories which have liquid chromatogram.
标题：超高压液相色谱法同时检测玉米中的伏马毒素B1、B2、B3
英文标题：Simultaneous determination of fumonisin B1, B2 and B3 in maize by ultra pressure liquid chromatography
作者：
王军淋 浙江工业大学化学工程与材料学院
胡玲玲 浙江工业大学化学工程与材料学院
蔡增轩 浙江省疾病预防控制中心
任一平 1.浙江工业大学化学工程与材料学院;2.浙江省疾病预防控制中心
中文关键词:超高压液相色谱法,伏马毒素,离子交换,邻苯二甲醛(OPA),萘-2,3-二甲醛(NDA),丹磺酰氯,6-氨基喹啉-N-羟基琥珀酰亚胺氨基甲酸酯(AQC),
英文关键词:ultra pressure liquid chromatography (UPLC),fumonisins,ion exchange,o-phthaldialdehyde (OPA),naphthalene-2,3-dicarboxaldehyde (NDA),dansyl chloride,6-Aminoquinolyl-N-Hydroxysuccinimidy-lcarbamate (AQC),
发表日期：2012-11-03
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