【摘要】：葉酸是一種B族維生素,對維持機(jī)體正常生理功能具有特殊的保障作用,然而市場上的葉酸產(chǎn)品質(zhì)量參差不齊,且多為合成產(chǎn)品,給消費(fèi)者的身體健康帶來隱患,也不利于監(jiān)管部門的質(zhì)量調(diào)控,主要原因就是質(zhì)量檢測方法的不規(guī)范和葉酸標(biāo)準(zhǔn)物質(zhì)的缺失。雙酚A作為一種重要的有機(jī)化工原料在我國被廣泛應(yīng)用,但產(chǎn)品質(zhì)量有待提高,且雙酚A產(chǎn)品中微量的雙酚A殘留正威脅著人們的身體健康,建立標(biāo)準(zhǔn)統(tǒng)一的質(zhì)量檢測方法及制備雙酚A標(biāo)準(zhǔn)物質(zhì)同樣刻不容緩。本文對葉酸及雙酚A的純化、定值方法進(jìn)行了詳細(xì)研究。本課題首先探究了采用浸提法提取、柱層析純化的方法從菠菜葉粉末中提取天然葉酸,通過單因素試驗(yàn)和正交設(shè)計(jì)試驗(yàn)考察了多種因素對提取效果的影響,并確定了最優(yōu)條件為:料液比為1:12,提取液為30 mmol/L的乙酸銨溶液,提取溫度為75℃,提取時(shí)間為30 min,柱層析吸附劑為硅膠,洗脫劑為二氯甲烷:甲醇=7:3(v/v),硅膠高度為10cm,上樣液體積為5 mL,最終的提取率為9.72μg/g。采用液-質(zhì)聯(lián)用法、紅外光譜法和核磁共振波譜法對實(shí)驗(yàn)室自制葉酸標(biāo)準(zhǔn)物質(zhì)進(jìn)行了定性分析,并進(jìn)行了定值分析。質(zhì)量平衡法測定純度為90.64%,與定量核磁法的測定結(jié)果90.57%相符,合成不確定度為0.13%,儲存在4℃條件下1個(gè)月可保持良好的穩(wěn)定性。為提高雙酚A純度,本課題通過制備型高效液相色譜法對純化工藝進(jìn)行了研究,確定純化條件為:原料濃度為20 mg/m L,流動(dòng)相為水:乙腈=65:35(v/v)等度洗脫程序,洗脫時(shí)間40 min,檢測波長為236 nm,流速為15 m L/min,進(jìn)樣量為2 m L,所得產(chǎn)品純度為99.92%,收率為21%,滿足標(biāo)準(zhǔn)物質(zhì)對純度的要求。通過液-質(zhì)聯(lián)用法、紅外光譜法和核磁共振波譜法對雙酚A原料進(jìn)行了定性分析。采用質(zhì)量平衡法對雙酚A原料的純度進(jìn)行了定值分析,測定結(jié)果為98.63%,合成不確定度為0.45%,儲存在4℃條件下1個(gè)月可保持良好的穩(wěn)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，

本文編號：2135906