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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 4μHydro-Rp-80a C18色谱柱(4.6 mm×250 mm,4μm),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(r~2)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。
Objective To establish a method for the determination of maleic acid in starch and starch products by solid phase extraction and high performance liquid chromatography. Methods After the sample was extracted with SAX solid phase extraction cartridge, the mobile phase was Synergi 4μHydro-Rp-80a C18 column (4.6 mm × 250 mm, 4 μm) and 0.1% CF3COOH solution (V: V) Effective separation of maleic acid from sample. Results The natural logarithm of peak area of maleic acid showed a good linear relationship with the natural logarithm of concentration. The correlation coefficient (r ~ 2) was 0.9998, the recovery was between 88.9% and 94.2%, and the relative standard deviation was 1.7 % To 2.9%, and the limit of detection (LOD) was 1.5 mg / kg (S / N = 3). Conclusion The method is fast and easy to operate, high accuracy and good reproducibility, which can meet the needs of actual detection.