本文選題：實(shí)施直接分析-質(zhì)譜法 + 熱輔助在線衍生化-氣相色譜法　； 參考：《浙江工業(yè)大學(xué)》2017年碩士論文

【摘要】：銀杏是我國(guó)特有的傳統(tǒng)植物,富含銀杏黃酮和萜內(nèi)酯等多種生物活性成分,具有很高的食、藥用價(jià)值,已被開發(fā)成各種保健品如銀杏茶、白果粉飲品等。本論文的研究對(duì)象為銀杏的主要毒性成分之一銀杏酸,具致敏性、細(xì)胞毒性和致突變毒性。歐盟和《中國(guó)藥典》分別規(guī)定銀杏葉提取物中銀杏酸含量不得超過5mg/kg和10 mg/kg,現(xiàn)行標(biāo)準(zhǔn)中雖未對(duì)銀杏保健品中的銀杏酸含量作出規(guī)定,但其攝入量不宜過多。為實(shí)現(xiàn)大批量銀杏保健品中銀杏酸的快速篩查和準(zhǔn)確定量,本論文開發(fā)了質(zhì)譜和色譜法用于銀杏飲品中銀杏酸的分析測(cè)定,具體研究成果總結(jié)如下:一、建立了實(shí)時(shí)直接分析-質(zhì)譜法(Direct Analysis in Real Time-Mass Spectrometry,DART-MS)對(duì)白果飲品中的銀杏酸進(jìn)行快速定性以及半定量分析的方法。研究影響離子化效率的因素,確定負(fù)離子模式、氦氣作為離子化氣體、樣品移動(dòng)速度0.2 mm/s、氣體溫度450℃為最優(yōu)條件,并進(jìn)行了方法學(xué)考察。該方法在2-50 mg/L濃度范圍內(nèi)線性良好,線性相關(guān)系數(shù)達(dá)0.9981,檢出限為0.5mg/L,RSD在12.5%-13.7%(n=6)之間,方法回收率為63.8%-71.2%。以GA13:0為外標(biāo),對(duì)銀杏葉、白果種仁、白果粉飲品中的銀杏酸進(jìn)行半定量分析并輔以二級(jí)質(zhì)譜定性,測(cè)得3種樣品中總銀杏酸含量分別為4799.4±545.3 mg/kg,67.4±10.9 mg/kg和26.6±2.3 mg/kg。將該法和熱輔助在線衍生化-氣相色譜法的方法學(xué)參數(shù)、定量結(jié)果進(jìn)行比較,誤差在合理范圍內(nèi),說明DART-MS法適用于銀杏酸的快速測(cè)定和半定量分析。憑借其快速、實(shí)時(shí)、前處理步驟少等優(yōu)點(diǎn),在大批量銀杏保健品中銀杏酸的快速篩查、定性以及半定量分析上顯示出強(qiáng)大的優(yōu)勢(shì)。二、建立了熱輔助在線衍生化-氣相色譜法(Thermochemolysis-Gas Chromatography,TMC-GC),用于銀杏保健品中銀杏酸的快速、準(zhǔn)確定量。采用甲醇對(duì)樣品粉末中的銀杏酸進(jìn)行萃取富集,萃取液與三甲基氫氧化硫(Trimethylsulfonium Hydroxide,TMSH)以1:2的比例在裂解爐300℃的高溫輔助下瞬間生成銀杏酸甲酯,由GC-FID(MS)分離測(cè)定,極大地提高了分析靈敏度。結(jié)果表明,銀杏酸GA13:0在5-600 mg/L濃度范圍內(nèi)線性良好,線性相關(guān)系數(shù)達(dá)0.9994,檢出限為1.8 mg/L(S/N=3),RSD為2.4%-2.6%(n=6)。以GA13:0為外標(biāo),分別測(cè)定白果種仁、白果粉飲品、銀杏葉、銀杏秋茶和春茶樣品中的7種銀杏酸,總含量在31.5 mg/kg-1.89×104 mg/kg之間。同時(shí),測(cè)定了銀杏秋茶和春茶中銀杏酸在沖泡90 min后的溶出率分別為16%和12%,溶出量分別為1.95mg/g和2.23 mg/g。白果粉飲品加標(biāo)回收率在87.1%-106.1%之間。本方法無(wú)需耗時(shí)的離線衍生化步驟,操作簡(jiǎn)便、定量準(zhǔn)確、靈敏度高,在DART-MS法快速篩查的基礎(chǔ)上,本法可進(jìn)一步應(yīng)用于大批量樣品中銀杏酸的準(zhǔn)確、快速定量。以上結(jié)果表明,本文開發(fā)的實(shí)時(shí)直接分析-質(zhì)譜法和熱輔助在線衍生化-氣相色譜法適于銀杏保健品中銀杏酸的分析研究,結(jié)果為銀杏保健品的快速篩查和質(zhì)量控制提供方法參考。
[Abstract]:Ginkgo biloba (Ginkgo biloba) is a unique traditional plant in China. It is rich in many bioactive components such as ginkgo flavonoids and terpene lactones and has high food and medicinal value. It has been developed into various health products such as ginkgo tea and white fruit powder drinks. In this paper, ginkgolic acid, one of the main toxic components of Ginkgo biloba, is studied, which is sensitive, cytotoxic and mutagenic. In EU and Chinese Pharmacopoeia, ginkgolic acid content in ginkgo biloba leaf extract should not exceed 5mg/kg and 10 mg / kg respectively. Although the current standard does not stipulate ginkgolic acid content in ginkgo biloba health products, its intake should not be excessive. In order to screen and quantify ginkgolic acid in large quantities of ginkgo health products, this paper developed mass spectrometry and chromatography for the determination of ginkgolic acid in ginkgo drinks. The specific research results are summarized as follows: 1. A real time direct Analysis in Real time Mass Spectrometry (DART-MS) method was developed for the rapid qualitative and semi-quantitative analysis of ginkgolic acid in ginkgo drinks. The factors affecting the efficiency of ionization were studied. The model of negative ion was determined. The helium as the ionizing gas, the moving speed of the sample was 0.2 mm / s, the temperature of the gas was 450 鈩，

本文編號(hào)：1996766