1.天津科技大学 食品营养与安全国家重点实验室,天津 300457
2.天津科技大学 天津市食品质量与健康 重点实验室,天津 300457
3.天津师范大学 生命科学学院,天津 300387
PAN Ming-fei,E-mail:panmf2012@tust.edu.cn
WANG Shuo,E-mail:s.wang@tust.edu.cn
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杨潇,杨晶莹,潘明飞等.沙棘果粉中异鼠李素和芦丁标准物质的制备与鉴定[J].分析测试学报,2022,41(05):682-691.
YANG Xiao,YANG Jing-ying,PAN Ming-fei,et al.Preparation and Identification of Reference Materials of Isorhamnetin and Rutin in Seabuckthorn Fruit Powder[J].Journal of Instrumental Analysis,2022,41(05):682-691.
杨潇,杨晶莹,潘明飞等.沙棘果粉中异鼠李素和芦丁标准物质的制备与鉴定[J].分析测试学报,2022,41(05):682-691. DOI: 10.19969/j.fxcsxb.21110206.
YANG Xiao,YANG Jing-ying,PAN Ming-fei,et al.Preparation and Identification of Reference Materials of Isorhamnetin and Rutin in Seabuckthorn Fruit Powder[J].Journal of Instrumental Analysis,2022,41(05):682-691. DOI: 10.19969/j.fxcsxb.21110206.
异鼠李素(IS)和芦丁(RU)是沙棘中存在的两种黄酮类化合物,具有很强的抗氧化活性,能有效清除体内的自由基。由于其在沙棘原料中含量低,还原性强,其标准品的制备和提纯难度较大。该研究采用乙醇溶解和高压液相制备相结合的方法制备了高纯度的IS和RU,并通过红外光谱、紫外光谱、质谱和核磁共振C/H谱进一步鉴定其化学结构。采用典型高效液相色谱法对获得的IS和RU产品的均一性(瓶内和瓶内)和稳定性(长期:6个月,-20 ℃;短期:1周,4 ℃和-20 ℃)进行验证。统计分析数据表明,IS和RU产品具有良好的均匀性和稳定性。采用多家实验室(,n, = 8)联合定值方式确定所制备的IS和RU标准物质的纯度分别为99.16%和99.22%,扩展不确定度分别为0.14%和0.13%。该研究获得的IS和RU标准物质可作参考物质用于药物分析或沙棘类产品的质量评价,具有良好的应用前景。该研究为沙棘中IS和RU标准物质的制备和质量验证提供了有效的方法,可推广应用于其他标准物质的制备过程。
Isorhamnetin(IS) and rutin(RU),two flavonoid compounds present in seabuckthorn,have very strong antioxidant activities for effective removal of free radicals in human body.In this paper,IS and RU of high-purity were prepared by a high-pressure liquid phase preparation method with ethanol dissolution,then their chemical structures were identified by Fourier transform infrared spectroscopy(FT-IR),ultraviolet(UV) spectroscopy,mass spectrometry(MS) and H/C-nuclear magnetic resonance(H/C-NMR).Furthermore,a typical HPLC method was used to evaluate the obtained IS and RU products in terms of homogeneity(inter and intra-bottles) and stability(long-term:6 months,-20 ℃;short-term:1 week,4 ℃ and -20 ℃),both of them were confirmed excellent by statistical data.Finally,the purities of the prepared IS and RU reference materials were jointly determined by multiple laboratories(,n, = 8) to be 99.16% and 99.22%,with their extended uncertainties of 0.14% and 0.13%,respectively.The IS and RU reference materials obtained in the study could be used as reliable references in drug analysis or quality evaluation on seabuckthorn products.This study provided an effective method for the preparation and identification of IS and RU reference materials in seabuckthorn,which could be applied to the preparation of other reference materials.
标准物质沙棘异鼠李素芦丁制备和验证
reference materialsseabuckthornisorhamnetinrutinpreparation and identification
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