固相萃取-高效液相色谱法测定淀粉及淀粉制品中顺丁烯二酸的含量

Determination of maleic acid in starch and starch products by solid phase extraction-high performance liquid chromatography

中文关键词:  顺丁烯二酸  顺丁烯二酸酐  固相萃取-高效液相色谱法  淀粉

英文关键词:maleic acid  maleic anhydride  solid phase extraction-high performance liquid chromatography  starch products

中文摘要:

      目的 建立固相萃取分离-高效液相色谱检测淀粉及淀粉制品中顺丁烯二酸含量的分析方法。方法 用SAX固相萃取小柱提取样品中的待测化合物后, 以Synergi 4 μ Hydro-Rp -80a C18色谱柱(4.6 mm × 250 mm, 4 μm), 0.1% CF3COOH溶液(V:V)为流动相, 有效分离样品中的顺丁烯二酸。结果 顺丁烯二酸色谱峰面积的自然对数与浓度的自然对数呈良好的线性关系, 相关系数(r2)为0.9998, 回收率在88.9%～94.2%之间, 相对标准偏差1.7%～2.9%, 检出限(LOD)为1.5 mg/kg(S/N=3)。结论 该法操作快速简单, 准确度高, 重现性好, 能够满足实际检测需要。

英文摘要:

      Objective To establish a method for the determination of maleic acid in starch and starch products by solid phase extraction-high performance liquid chromatography. Methods A SAX solid phase extraction column was used to extract the analytes from the samples. The maleic acid in the sample was effectively separated on a Synergi 4 μ Hydro-Rp-80a C18 column (4.6 mm×250 mm, 4 μm), using 0.1% CF3COOH (V:V) as the mobile phase. Results The natural logarithm of chromatographic peak area and concentration had a good linear relationship (r2>0.9998). The results indicated that the limit of quantification (LOD) of maleic acid was 1.5 mg/kg (S/N=3). The recoveries of maleic acid from spiked samples were ranged from 88.9% to 94.2% with RSDs of 1.7%~2.9% (n=6). Conclusion The method is simple, precise and had high recoveries for the determination of maleic acid in actual samples.