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        救必應(yīng)酸的單體制備及RP—HPLC法測(cè)定救必應(yīng)藥材及精制品中3種活性成分的含量

        發(fā)布時(shí)間:2019-08-30 來源: 人生感悟 點(diǎn)擊:


          中圖分類號(hào) R284.1 文獻(xiàn)標(biāo)志碼 A 文章編號(hào) 1001-0408(2018)03-0326-04
          DOI 10.6039/j.issn.1001-0408.2018.03.09
          摘 要 目的:制備高純度的救必應(yīng)酸并測(cè)定救必應(yīng)藥材及精制品中3種活性成分紫丁香苷、長(zhǎng)梗冬青苷、救必應(yīng)酸的含量。方法:采用醇提法制備救必應(yīng)皂苷,以甲醇和氫氧化鈉進(jìn)一步水解,并經(jīng)重結(jié)晶后得到救必應(yīng)酸單體。采用反相高效液相色譜(RP-HPLC)法測(cè)定救必應(yīng)藥材及精制品1和精制品2中紫丁香苷、長(zhǎng)梗冬青苷、救必應(yīng)酸的含量。色譜柱為Agilent XDB C18,流動(dòng)相為水-乙腈(梯度洗脫),柱溫為30 ℃,流速為1.2 mL/min,檢測(cè)波長(zhǎng)為210 nm,進(jìn)樣量為10 μL。結(jié)果:所制救必應(yīng)酸純度達(dá)99%以上。紫丁香苷、長(zhǎng)梗冬青苷、救必應(yīng)酸進(jìn)樣量分別在0.18~3.22、0.59~10.36、0.20~3.53 μg范圍內(nèi)與各自峰面積積分值呈良好線性關(guān)系(r均為0.999 9),精密度、穩(wěn)定性(24 h)、重復(fù)性試驗(yàn)的RSD均小于2.0%(n=6~7),平均加樣回收率為96.08%~100.81%(RSD≤1.98%,n=6)。紫丁香苷、長(zhǎng)梗冬青苷、救必應(yīng)酸的含量在救必應(yīng)藥材中分別為1.61%、7.26%、1.29%(RSD≤1.08%,n=3),在精制品1中分別為0、82.59%、4.18%(RSD≤1.67%,n=3);在精制品2中分別為0、73.29%、7.41%(RSD≤1.15%,n=3)。結(jié)論:所制救必應(yīng)酸純度高、制備方法簡(jiǎn)單且安全環(huán)保。建立的RP-HPLC法簡(jiǎn)單、可靠,可滿足快速測(cè)定救必應(yīng)藥材及其精制品含量的要求。
          關(guān)鍵詞 救必應(yīng);紫丁香苷;長(zhǎng)梗冬青苷;救必應(yīng)酸;制備;反相高效液相色譜法
          ABSTRACT OBJECTIVE: To prepare high-purity rotundic acid, and to determine the contents of syringoside, peduncloside and rotundic acid in Ilicis rotundae and its refined products. METHODS: I. rotundae saponins was prepared by ethanol extraction method and hydrolyzed with methanol and sodium hydroxide; rotundic acid monomer was obtained after recrystallization. The contents of syringoside, peduncloside and rotundic acid in I. rotundae, its refined product 1 and its refined product 2 were determined by RP-HPLC. The determination was performed on an Agilent XDB C18 column with mobile phase consisted of water-acetonitrile (gradient elution) at the flow rate of 1.2 mL/min. The column temperature was 30 ℃, and the detection wavelength was set at 210 nm. The sample size was 10 μL. RESULTS: The purity of rotundic acid exceeded 99%. The linear ranges of syringing, peduncloside and rotundic acid were 0.18-3.22, 0.59-10.36 and 0.20-3.53 μg, respectively (r=0.999 9). RSDs of precision, stability (24 h) and reproducibility tests were all lower than 2.0% (n=6-7). The average recoveries were 96.08%-100.81%(RSD≤1.98%,n=6). The contents of syringoside, peduncloside and rotundic acid in I. rotundae were 1.61%, 7.26%, 1.29% (RSD≤1.08%, n=3); those of refined product 1 were 0, 82.59%, 4.18% (RSD≤1.67%, n=3); those of refined product 2 were 0, 73.29%, 7.41% (RSD≤1.15%,n=3), respectively. CONCLUSIONS: Prepared rotundic acid has high purity and is simple in preparation, safe and environmentally-friendly. RP-HPLC method that established is simple and reliable, and can meet the requirements for rapid analysis of I. rotundae and its refined products.
          KEYWORDS Ilicis rotundae; Syringoside; Peduncloside; Rotundic acid; Preparation; RP-HPLC

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