本文選題：逆三相膜萃取　切入點：尼古丁　出處：《新疆醫(yī)科大學》2017年碩士論文　論文類型：學位論文

【摘要】：目的:建立逆三相膜萃取生物堿(尼古丁及氧化槐果堿),利用高效液相色譜法(HPLC)和紫外-可見分光光度法(UV)對提取物尼古丁和氧化槐果堿進行定性定量分析。方法:1.聚四氟乙烯膜(PTFE)作為萃取膜,有機溶劑為氯仿,水相和有機相體積比2.5∶1,0.01mol/L硫酸作為酸相萃取劑,1.25mol/L氫氧化鈉作為堿相萃取劑,流速6mL/min,萃取時間25min。2.在單因素試驗的基礎上,采用L16(45)正交試驗進一步考察條件,水相和有機相體積比為1∶1,0.3mol/L鹽酸作為酸相萃取劑,0.75mol/L氫氧化鈉作為堿相萃取劑,流速6mL/min、萃取時間60min。由直觀分析可知,選取鹽酸濃度(A)、氫氧化鈉濃度(B)、提取時間(C)、體積比(D)4個因素,設計每個因素選取4個水平時,最佳提取工藝為A2B3C4D1,以鹽酸濃度影響最大。結果:1.最佳實驗條件下,尼古丁在25min內(nèi)萃取率達到99.07%;高效液相色譜法定性定量分析尼古丁時色譜柱為C18柱(259mm×4.6mm),流動相為甲醇-0.2%磷酸水溶液(10∶90),進樣量為10μL,柱溫25℃,檢測波長261nm,回歸方程:Y=34014X+225.23,(r=0.9995,n=6),0.01~0.35μg/m L范圍內(nèi)線性關系良好,精密度RSD為0.98%,穩(wěn)定性RSD為1.16%,重復性RSD為0.67%,平均加樣回收率為99.26%。伊犁、巴楚、山東、庫車和和田等五種產(chǎn)地1g煙草葉中尼古丁含量分別為24.43mg、23.12mg、21.39mg、13.72mg和5.93mg,伊犁煙草葉中尼古丁含量最高;2.最佳條件下氧化槐果堿在60min內(nèi)萃取率達到98.21%。高效液相色譜法測定條件:Shim-packVP-ODS色譜柱(250mm×4.6mm,5μm),流動相為甲醇-0.2%磷酸水溶液(7∶93),梯度洗脫,流速1mL/min,進樣量5μL,柱溫30℃,檢測波長221nm,在0.01~0.7mg/mL范圍內(nèi)線性關系良好,回歸方程為Y=1610.90X-190.06,(r=0.9978,n=6),精密度RSD為0.93%,穩(wěn)定性RSD為0.88%,重復性RSD為1.88%,平均回收率為97.35%。結論:1.通過逆三相膜循環(huán)萃取分離系統(tǒng),萃取的尼古丁和氧化槐果堿純度高、操作簡單、有機溶劑消耗量低等特點,可用于其他生物堿、皂苷類和稀土金屬離子的提取分離。
[Abstract]:Objective: to establish an inverse three-phase membrane extraction of alkaloids (nicotine and oxysophorine), and to determine the qualitative and quantitative analysis of nicotine and oxysophorine by high performance liquid chromatography (HPLC) and ultraviolet-visible spectrophotometry (UV). Polytetrafluoroethylene (PTFE) as an extraction membrane, The organic solvent is chloroform, the volume ratio of aqueous phase to organic phase is 2.5: 10.01mol / L sulfuric acid as acid phase extractant 1.25mol / L sodium hydroxide as alkali phase extractant, the flow rate is 6ml / min, the extraction time is 25min. 2. On the basis of single factor test, the conditions for further investigation are further investigated by L1645 orthogonal test. The volume ratio of hydrochloric acid to organic phase is 1: 1 / 1, 0.3 mol / L hydrochloric acid is used as acid phase extractant 0.75 mol / L sodium hydroxide as alkali phase extractant, the flow rate is 6 mL / min and the extraction time is 60 min. When each factor was selected at 4 levels, the optimum extraction process was A 2B 3C 4D 1, the concentration of hydrochloric acid was the most important. The extraction rate of nicotine reached 99.07% in 25 min, the chromatographic column for quantitative analysis of nicotine was C18 column (259mm 脳 4.6 mm), the mobile phase was methanol-0.2% phosphoric acid solution (10: 90m), the sample quantity was 10 渭 L, and the column temperature was 25 鈩，

本文編號：1622862