【摘 要】
:
采用HPLC-ESI-MS/MS联用技术,检测淀粉及其制品中马来酸残留量。样品经50%水-50%甲醇提取后,以C18柱为液相分离柱,以甲醇和1%甲酸为流动相,多反应监测模式测定马来酸,其定性
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采用HPLC-ESI-MS/MS联用技术,检测淀粉及其制品中马来酸残留量。样品经50%水-50%甲醇提取后,以C18柱为液相分离柱,以甲醇和1%甲酸为流动相,多反应监测模式测定马来酸,其定性定量离子对分别为114.9/71.0。马来酸含量在10~100ng/mL范围内具有良好的线性关系,测定下限(10S/N)为10ng/mL。以淀粉为基体,加入3种不同浓度水平的马来酸做加标回收试验,回收率在85%~100%,相对标准偏差(n=6)小于10%。该方法操作简单,结果准确,重现性好。
The residues of maleic acid in starch and its products were determined by HPLC-ESI-MS / MS. After the sample was extracted with 50% water-50% methanol, C18 column was used as the liquid phase separation column. The mobile phase consisted of methanol and 1% formic acid as the mobile phase. The multi-reaction monitoring mode was used to determine maleic acid. The qualitative and quantitative ion pairs were 114.9 / 71.0 . The maleic acid content has a good linear relationship in the range of 10 ~ 100ng / mL, and the lower limit of determination (10S / N) is 10ng / mL. The recoveries of 85% ~ 100% with relative standard deviation (n = 6) of less than 10% were obtained by adding spiked maleic acid with 3 different concentrations of starch as matrix. The method is simple, accurate and reproducible.
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