多指标综合平衡正交实验设计法优化液相色谱分析饮料中食品添加剂的操作条件

Multi-index and synthetical balanced orthogonal experimental design optimized the liquid chromatography operation conditions in analysis of food additives in drinks

目的优化液相色谱法分析儿童饮料中安赛蜜、糖精钠、苯甲酸和山梨酸操作条件。方法利用多指标综合平衡正交实验设计法,综合分析柱温、进样体积和柱流量3个因素和3个水平对色谱保留时间、峰面积和分离度3个指标的影响程度。结果确定了最佳的操作条件:使用BDS HYPERSIL C18色谱柱(150 mm×4.6 mm,5μm),以乙腈和磷酸二氢钾溶液为流动相,采用梯度洗脱程序,保持柱流量1.500 ml/min,柱温40℃,进样体积10μl,各组分最大吸收波长作为检测波长。结论采用正交实验设计优化后的色谱分离条件,能够达到出峰快、检出限低和分离度好的目的,该方案能够科学地反映各因素对各指标的影响程度,从而有侧重地改善某个指标的分离效果,易于实际应用。

[Objective]To optimize the operation condition of liquid chromatography in analysis of acesulfame-K,saccharin sodium,benzoic acid and sorbic acid in children drinks.[Methods]The influence of three factors（column temperature,injection volume and column flow）in three levels on three indexes（retention time,peak area and resolution）was analyzed by multi-index and synthetical balanced orthogonal experimental design.[Results]The optimum operation conditions were determined：BDS HYPERSIL C18 chromatographic column（150 mm×4.6 mm,5 μm）,methyl cyanide and potassium dihydrogen phosphate solution were as mobile phase,the gradient elution chromatography was adopted,Column flow was 1.500 ml/min,column temperature was40 ℃,injection volume was 10 μl,and the maximum absorption wavelength of the four target material was as the testing wavelength.[Conclusion]The chromatographic separation conditions which were optimized by the orthogonal experimental design can realize the objectives as followed：the high efficiency,the lower detection limit and the better resolution. This method can reflect the influence of each factor on each index scientifically,so that we could put particular emphasis on improving some index and make it easy to use.