離子色譜分離保留因子計算定性分析低聚殼寡糖的研究
發(fā)布時間:2018-04-27 08:25
本文選題:低聚殼寡糖 + 殼聚糖; 參考:《藥物分析雜志》2017年01期
【摘要】:目的:建立陰離子交換色譜分離,并用保留因子計算法定性分析低聚殼寡糖。方法:首先利用高效陰離子交換色譜-積分脈沖安培檢測法(HPAEC-IPAD)對5種殼寡糖(聚合度DP=2~6)標準樣品進行分離;分離條件:采用DIONEX CarboPac·PA10(4.0 mm×50 mm)保護柱和DIONEX CarboPac·PA10(4.0 mm×250mm)分析柱,淋洗液采用氫氧化鈉溶液,積分脈沖安培法檢測。然后用建立的分離方法對殼寡糖樣品進行分離并定性。再根據(jù)所得樣品色譜峰的保留時間分別計算保留因子,建立殼寡糖聚合度(DP)與其保留因子(k')的相關(guān)關(guān)系,根據(jù)建立的相關(guān)關(guān)系對未知的殼寡糖進行定性,并用質(zhì)譜方法對未知殼寡糖樣品進行驗證。結(jié)果:殼寡糖聚合度的對數(shù)值與其保留因子的對數(shù)值具有線性關(guān)系,回歸系數(shù)R~2≥0.998 7,利用建立的線性回歸方程對樣品中的4種未知殼寡糖樣品的定性結(jié)果為殼七糖、殼八糖、殼九糖和殼十糖,誤差≤5.66%。質(zhì)譜方法對未知殼寡糖樣品進行了驗證,驗證結(jié)果為樣品中存在殼二糖、殼三糖、殼四糖、殼五糖、殼六糖、殼七糖和殼八糖。結(jié)論:對于殼寡糖樣品用離子色譜分離,保留因子計算來定性殼寡糖聚合度的方法是可行的。
[Abstract]:Objective: to establish anionic exchange chromatography and to calculate the legal analysis of oligochitosan oligosaccharides with retention factors. Methods: first, 5 kinds of chitosan oligosaccharides (DP=2~6) standard samples were separated by high performance anion exchange chromatography - integrated pulse amperometric detection (HPAEC-IPAD), and the separation conditions were: using DIONEX CarboPac. PA10 (4 mm x 50 mm). The column and DIONEX CarboPac PA10 (4 mm x 250mm) column were analyzed with sodium hydroxide solution and integrated pulse ampere method. Then the chitosan oligosaccharide samples were separated and qualitatively separated by the established separation method. The retention factors were calculated according to the retention time of the chromatographic peaks, and the degree of polymerization of chitosan oligosaccharides (DP) and their retention were established. The correlation relation of factor (k'), the unknown shell oligosaccharides are qualitatively determined according to the relationship established, and the samples of the unknown shell oligosaccharides are verified by mass spectrometry. Results: the value of the degree of polymerization of the oligosaccharide oligosaccharides has a linear relationship with the value of the retention factor, the regression coefficient R~2 is more than 0.9987, and the linear regression equation established to the sample is used for the sample. The qualitative results of 4 uncharted oligosaccharides were shell seven sugar, shell eight sugar, shell nine sugar and shell ten sugar. The samples of unknown shell oligosaccharides were verified by error less than 5.66%. mass spectrometry. The results showed that there were shell two sugar, shell three sugar, shell four sugar, shell five sugar, shell six sugar, shell seven sugar and shell eight sugar. It is feasible to determine the degree of polymerization of chitosan oligosaccharides by spectral separation and retention factor calculation.
【作者單位】: 浙江樹人大學(xué)生物與環(huán)境工程學(xué)院;
【基金】:浙江省自然科學(xué)重點基金(編號:Z14B070001) 浙江省分析測試基金(編號:2015C37039)
【分類號】:R917
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