建立黄精酵素口服液中金属元素形态分析的方法。用0.45μm微孔滤膜将黄精口服液中金属元素分为悬浮态和可溶态,用D101大孔吸附树脂将可溶态分为无机态和有机态,分别用丙酮和无水乙醇将有机态中的蛋白结合态和多糖结合态分离出来,试验选择微波消解-HR-CS FAAS法测定各形态中Ca、Fe、Zn。结果表明:黄精酵素口服液中Ca、Fe、Zn含量丰富,分别为318.80±5.38μg/m L、17.93±0.28μg/m L、3.50±0.06μg/m L,多以可溶态形式存在。可溶态中主要以有机态为主,Ca、Fe、Zn的有机态分别达到总量的54.11%、49.74%、55.40%,蛋白结合态分别达到总量的16.24±0.39%、12.42±0.22%、13.21±0.29%,多糖结合态分别达到总量的25.07±0.50%、18.47±0.28%、4.35±0.29%,除了Zn的多糖结合态所占比例较小,其他的都很高。该方法具有较高的实用价值,为金属元素形态分析提供科学依据和进一步研究黄精酵素口服液的功能提供基础数据。
A method was developed for the speciation analysis of metal elements in the oral liquid containing Polygonatum and enzymes. The suspended or soluble metals in the oral liquid were isolated by using a 0.45-μm microporous membrane. The inorganic and organic metal species were purified with a D101 macroporous adsorption resin, and the protein-bound and polysaccharide-bound metals were separated from the organic metal species by acetone and absolute ethyl alcohol extractions, respectively. Microwave digestion-high resolution continuum source flame atomic absorption spectrometry(HR-CS FAAS) was used to determine calcium, iron and zinc in different species. The results showed that there were high contents of calcium(318.80 ± 5.38 μg/m L), iron(17.93 ± 0.28 μg/m L), and zinc(3.50 ± 0.06 μg/m L) in the oral liquid containing Polygonatum and enzymes, and most of these metal elements were soluble. Organic metal species were dominant among the soluble metal elements, with organic calcium, iron, and zinc elements accounting for 54.11%, 49.74%, and 55.40%, respectively, of the corresponding total metal elements in the oral liquid. Protein-bound calcium, iron, and zinc accounted for 16.24 ± 0.39%, 12.42 ± 0.22%, and 13.21 ± 0.29%, respectively, of the corresponding total metal elements in the oral liquid. Polysaccharide-bound calcium, iron, and zinc accounted for 25.07 ± 0.50%, 18.47 ± 0.28%, and 4.35 ± 0.29%, respectively, of the corresponding total metal elements in the oral liquid, showing that the polysaccharide-bound zinc content was lower than that of the other metal species. The proposed method shows a high practical value, providing a scientific basis for the speciation analysis of metal elements and illustrating fundamental data for further study on the functions of the oral liquid containing Polygonatum and enzymes.