叶酸与双酚A的纯化定值研究
发布时间：2018-07-21 15:03
【摘要】：叶酸是一种B族维生素,对维持机体正常生理功能具有特殊的保障作用,然而市场上的叶酸产品质量参差不齐,且多为合成产品,给消费者的身体健康带来隐患,也不利于监管部门的质量调控,主要原因就是质量检测方法的不规范和叶酸标准物质的缺失。双酚A作为一种重要的有机化工原料在我国被广泛应用,但产品质量有待提高,且双酚A产品中微量的双酚A残留正威胁着人们的身体健康,建立标准统一的质量检测方法及制备双酚A标准物质同样刻不容缓。本文对叶酸及双酚A的纯化、定值方法进行了详细研究。本课题首先探究了采用浸提法提取、柱层析纯化的方法从菠菜叶粉末中提取天然叶酸,通过单因素试验和正交设计试验考察了多种因素对提取效果的影响,并确定了最优条件为:料液比为1:12,提取液为30 mmol/L的乙酸铵溶液,提取温度为75℃,提取时间为30 min,柱层析吸附剂为硅胶,洗脱剂为二氯甲烷:甲醇=7:3(v/v),硅胶高度为10cm,上样液体积为5 mL,最终的提取率为9.72μg/g。采用液-质联用法、红外光谱法和核磁共振波谱法对实验室自制叶酸标准物质进行了定性分析,并进行了定值分析。质量平衡法测定纯度为90.64%,与定量核磁法的测定结果90.57%相符,合成不确定度为0.13%,储存在4℃条件下1个月可保持良好的稳定性。为提高双酚A纯度,本课题通过制备型高效液相色谱法对纯化工艺进行了研究,确定纯化条件为:原料浓度为20 mg/m L,流动相为水:乙腈=65:35(v/v)等度洗脱程序,洗脱时间40 min,检测波长为236 nm,流速为15 m L/min,进样量为2 m L,所得产品纯度为99.92%,收率为21%,满足标准物质对纯度的要求。通过液-质联用法、红外光谱法和核磁共振波谱法对双酚A原料进行了定性分析。采用质量平衡法对双酚A原料的纯度进行了定值分析,测定结果为98.63%,合成不确定度为0.45%,储存在4℃条件下1个月可保持良好的稳定性。
[Abstract]:Folic acid is a B group vitamin, which has a special function to maintain the normal physiological function of the body. However, the quality of folic acid products on the market is uneven, and most of them are synthetic products, which bring hidden dangers to the health of consumers. The main reasons are the nonstandard quality detection method and the deficiency of folic acid standard material. Bisphenol A (BPA) is widely used as an important organic chemical raw material in China, but the product quality needs to be improved, and the microamounts of bisphenol A residues in bisphenol A products are threatening people's health. It is also urgent to establish a unified quality detection method and to prepare bisphenol A standard material. The purification and determination of folic acid and bisphenol A were studied in detail. In this paper, the extraction of natural folic acid from spinach leaf powder by extraction and column chromatography was studied. The influence of many factors on the extraction effect was investigated by single factor experiment and orthogonal design experiment. The optimum conditions are as follows: the ratio of solid to liquid is 1: 12, the extraction solution is 30 mmol / L ammonium acetate solution, the extraction temperature is 75 鈩，
本文编号：2135906
[Abstract]:Folic acid is a B group vitamin, which has a special function to maintain the normal physiological function of the body. However, the quality of folic acid products on the market is uneven, and most of them are synthetic products, which bring hidden dangers to the health of consumers. The main reasons are the nonstandard quality detection method and the deficiency of folic acid standard material. Bisphenol A (BPA) is widely used as an important organic chemical raw material in China, but the product quality needs to be improved, and the microamounts of bisphenol A residues in bisphenol A products are threatening people's health. It is also urgent to establish a unified quality detection method and to prepare bisphenol A standard material. The purification and determination of folic acid and bisphenol A were studied in detail. In this paper, the extraction of natural folic acid from spinach leaf powder by extraction and column chromatography was studied. The influence of many factors on the extraction effect was investigated by single factor experiment and orthogonal design experiment. The optimum conditions are as follows: the ratio of solid to liquid is 1: 12, the extraction solution is 30 mmol / L ammonium acetate solution, the extraction temperature is 75 鈩，
本文编号：2135906
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