造紙法再造煙葉萃取液與濃縮液含水率的測定研究
發(fā)布時(shí)間:2019-08-26 來源: 人生感悟 點(diǎn)擊:
摘 要:通過對色譜條件和前處理?xiàng)l件的選擇優(yōu)化,建立了造紙法再造煙葉萃取液和濃縮液含水率準(zhǔn)確、快速測定的氣相色譜法。再造煙葉萃取液或濃縮液樣品經(jīng)乙醇振蕩萃取過濾后,采用氣相色譜結(jié)合熱導(dǎo)檢測器(TCD)進(jìn)行含水率的測定。結(jié)果表明:方法線性范圍為1.00~16.00mg/mL,R2=0.9999,加標(biāo)回收率在96.7%~101.8%,檢出限和定量限分別為0.05mg/mL、0.16mg/mL,萃取液和濃縮液測定的RSD分別為0.1% 、0.4% (n=6)。該方法可消除煙草萃取液和濃縮液中易揮發(fā)性成分對含水率測定的影響,是一種簡單、快速、準(zhǔn)確可靠的方法。
關(guān)鍵詞:再造煙葉;萃取液;濃縮液;含水率;氣相色譜法
中圖分類號 S572 文獻(xiàn)標(biāo)識碼 A 文章編號 1007-7731(2019)01-0106-05
Quantifying Moisture Content in Liquid Extracts and Concentrated Solutions in Paper-making Reconstituted Tobacco
Wang Hua1 et al.
。1Technology center of China Tobacco Anhui Industrial Corporation,Hefei 230088,China)
Abstract:A rapid and accurate quantitative analysis method of moisture content in liquid extracts and concentrated solutions by GC was established on the basis of the main parameters affecting such as chromatographiccondition and Pretreatment conditions were optimized.The water content in liquid extracts and concentrated solutions samples were extracted with ethanol oscillation,after
filtered by 0.45μm organic membrane,then determinations were performed by GC with TCD detector and quantified by internal standard method.The results showed that The linear range of the method was 1.00-16.00mg/mL with R2 of 0.9999,the recovery ranged from 96.7 % to 101.8 %,and the detection limit and the limit of quantification were 0.05mg/mL and 0.16mg/mL ,the liquid extracts and concentrated solutions relative standard deviations(RSDs) were 0.1 % (n=6) and 0.4 % (n=6) ,respectively.This method simple,rapid,accurate,which can eliminates the errors caused by volatile components in liquid extracts and concentrated solutions in the determination of moisture content,andoffered more accurate and reliable results.
Key words:Reconstituted tobacco;Liquid extract;Concentrated solution;Moisture content;Gas chromatographic method
造紙法再造煙葉萃取液或濃縮液由水和固形物2個(gè)部分組成,其含水率指標(biāo)可間接反映固形物含量的大小。再造煙葉萃取液和濃縮液中的固形物含量是濃縮工序質(zhì)量控制的核心指標(biāo),也是造紙法再造煙葉過程和成品品質(zhì)控制的關(guān)鍵參數(shù)。但目前萃取液或濃縮液中固形物含量的測定方法均存在一些缺陷[1],根據(jù)再造煙葉萃取液和濃縮液的成分組成,要準(zhǔn)確測定其中的固形物含量,可通過測定樣品含水率來實(shí)現(xiàn)。
目前,含水率的測定方法主要有熱干燥法[2]、烘箱法[3]、蒸餾法[4]、卡爾費(fèi)休法[5-8]、核磁共振法[9]、近紅外光譜法[10]等。然而,上述方法均存在一些缺點(diǎn)。例如:在熱干燥法和烘箱法的實(shí)際溫度下,所失去的是揮發(fā)性物質(zhì)的總量,而不完全是水分;在蒸餾法復(fù)雜體系中,水與有機(jī)溶劑易發(fā)生乳化現(xiàn)象,樣品中的水分可能未完全揮發(fā)出來,水分有時(shí)附著在冷凝管壁上,造成讀數(shù)誤差;卡爾費(fèi)休法消耗試劑多、操作繁瑣;近紅外光譜法需要先建模,但建模的難度較大,定標(biāo)樣品的選擇、制備,精確的化學(xué)分析,基礎(chǔ)數(shù)據(jù)的準(zhǔn)確性以及選擇計(jì)量學(xué)方法的合理性,都將直接影響最終的分析結(jié)果。氣相色譜法(GC)則能夠消除揮發(fā)性成分對含水率測定結(jié)果的影響[11],具有快速、靈敏、準(zhǔn)確等優(yōu)點(diǎn),現(xiàn)已廣泛用于中藥[12]及煙草[13-15]含水率的測定。但目前有關(guān)氣相色譜測定再造煙葉萃取液和濃縮液含水率的研究尚未見報(bào)道。為此,本研究針對上述分析方法的不足,建立了測定再造煙葉萃取液和濃縮液含水率的氣相色譜法,為再造煙葉固形物含量的準(zhǔn)確測定奠定基礎(chǔ)。
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