Comparison of Six Sample Preparation Methods for Analysis of Food Additives in Milk Powder

Comparison of Six Sample Preparation Methods for Analysis of Food Additives in Milk Powder
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奶粉中食品添加剂分析六种样品制备方法的比较

DOI:
10.1007/s12161-013-9756-8
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发表时间:
2014-07
影响因子:
2.9
通讯作者:
Hou Xiaofang
Hou Xiaofang
中科院分区:
农林科学3区
文献类型:
--
作者:
Ma Jing;Zhang Bing;Wang Yunan;Hou Xiaofang

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奶粉基质是高度复杂的,含有大量的脂质和蛋白质;因此,在仪器分析之前,测定其中的痕量残留物和污染物通常需要大量的样品提取和制备。理想的制备方法是简单、耗时少且相对便宜。它提高了回收率,并涉及有毒有机溶剂的低消耗。本研究建立了六种奶粉样品前处理方法,包括液液萃取法、有机沉淀法、重沉淀法和三种不同的固相萃取法,并进行了比较。提取回收率进行了评估,通过测定6个防腐剂和甜味剂(苯甲酸,山梨酸,纳他霉素,溶菌酶,糖精钠,和糖精钠),由HPLC-DAD在整个和脱脂奶粉样品。结果表明,液-液萃取法的回收率在80%以上,但重现性不如固相萃取法;有机沉淀法和重沉淀法的回收率较低(低于20%); HLB柱的回收率最高(> 85%),而C18柱和MAX柱的回收率最低(> 85%)。因此,选择HLB柱作为HPLC-DAD法测定奶粉样品中6种防腐剂和甜味剂的最佳样品前处理材料。
Milk powder matrix is highly complex with significant amounts of lipids and proteins; thus, the determination of trace residues and contaminants in it often requires extensive sample extraction and preparation prior to instrumental analysis. An ideal preparation method is simple, less time consuming, and relatively inexpensive. It enhances the recovery and involves low consumption of toxic organic solvents. In this study, six sample preparation methods for milk powder were established and compared, including liquid–liquid extraction, organic precipitation, heavy precipitation, and three different solid-phase extraction (SPE) methods. The extraction recovery was evaluated by determination of six preservatives and sweeteners (benzoic acid, sorbic acid, natamycin, lysozyme, saccharin sodium, and aspartame) by HPLC-DAD in whole and skimmed milk powder samples. The results showed that the reproducibility of liquid–liquid extraction was not as high as the SPE method although the recovery was beyond 80 %; the organic precipitation and heavy precipitation gave poor recovery (below 20 %) of lysozyme; the highest recovery (>85 %) was achieved using the HLB cartridge compared to C18 and MAX cartridges. Therefore, the HLB cartridge was selected as the most appropriate sample preparation material for the determination of the six preservatives and sweeteners in milk powder samples by HPLC-DAD.
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