造纸法再造烟叶萃取液与浓缩液含水率的测定研究
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摘要
通过对色谱条件和前处理条件的选择优化,建立了造纸法再造烟叶萃取液和浓缩液含水率准确、快速测定的气相色谱法。再造烟叶萃取液或浓缩液样品经乙醇振荡萃取过滤后,采用气相色谱结合热导检测器(TCD)进行含水率的测定。结果表明:方法线性范围为1.00～16.00mg/mL,R2=0.9999,加标回收率在96.7%～101.8%,检出限和定量限分别为0.05mg/mL、0.16mg/mL,萃取液和浓缩液测定的RSD分别为0.1%、0.4%(n=6)。该方法可消除烟草萃取液和浓缩液中易挥发性成分对含水率测定的影响,是一种简单、快速、准确可靠的方法。
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 were0.05mg/mL and 0.16mg/mL,the liquid extracts and concentrated solutions relative standard deviations(RSDs)were0.1 %(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.
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 were0.05mg/mL and 0.16mg/mL,the liquid extracts and concentrated solutions relative standard deviations(RSDs)were0.1 %(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.
引文
[1]黄兰,葛少林,汪华,等.造纸法再造烟叶萃取液与浓缩液固形物含量的测定[J].烟草科技,2018,51(10):64-70.
[2]GB/T 2007.6-1987散装矿产品取样、制样通则水分测定方法-热干燥法[S].
[3]YC/T 31-1996烟草及烟草制品试样的制备和水分的测定烘箱法[S].
[4]GB/T 8929-2006原油水含量的测定蒸馏法[S].
[5]GB/T 8570.5-2010液体无水氨的测定方法第5部分:水分卡尔·费休法[S].
[6]GB/T 26626-2011/ISO 8534:2008动植物油脂水分含量测定卡尔·费休法(无吡啶)[S].
[7]GB/T 6283-2008化工产品中水分含量的测定卡尔·费休法(通用方法)[S].
[8]叶丹丹,王晓静,罗梅杰,等.卡尔费休法测定润滑油产品中的含水量[J].石化技术,2018(8):101-102.
[9]魏硕,王德勋,苏家恩,等.低场核磁共振法测定烘烤过程中烤烟主脉的水分[J].烟草科技,2016,49(10):31-35.
[10]李水芳,张欣,单杨,等.近红外光谱检测蜂蜜中可溶性固形物含量和水分的应用研究[J].光谱学与光谱分析,2010,30(9):2377-2380.
[11]史训瑶,杨小勇,左闻宇,等.烘箱法及气相色谱法测定烟叶水分及其差异分析[J].广东化工,2015,42(23):193-194.
[12]贾敏鸽,王燕,许丹,等.中药丸剂中水分的GC法测定[J].药物分析杂志,2004,24(6):616-619.
[13]GB/T 23203.1-2013卷烟总粒相物中水分的测定第1部分:气相色谱法[S].
[14]伍锦鸣,彭斌,刘克建,等.气相色谱法测定烟草含水率[J].烟草科技,2012(12):49-51.
[15]YC/T 345-2010烟草及烟草制品水分的测定气相色谱法[S].
[16]GB/T 6682-2008分析实验室用水规格和试验方法[S].
[2]GB/T 2007.6-1987散装矿产品取样、制样通则水分测定方法-热干燥法[S].
[3]YC/T 31-1996烟草及烟草制品试样的制备和水分的测定烘箱法[S].
[4]GB/T 8929-2006原油水含量的测定蒸馏法[S].
[5]GB/T 8570.5-2010液体无水氨的测定方法第5部分:水分卡尔·费休法[S].
[6]GB/T 26626-2011/ISO 8534:2008动植物油脂水分含量测定卡尔·费休法(无吡啶)[S].
[7]GB/T 6283-2008化工产品中水分含量的测定卡尔·费休法(通用方法)[S].
[8]叶丹丹,王晓静,罗梅杰,等.卡尔费休法测定润滑油产品中的含水量[J].石化技术,2018(8):101-102.
[9]魏硕,王德勋,苏家恩,等.低场核磁共振法测定烘烤过程中烤烟主脉的水分[J].烟草科技,2016,49(10):31-35.
[10]李水芳,张欣,单杨,等.近红外光谱检测蜂蜜中可溶性固形物含量和水分的应用研究[J].光谱学与光谱分析,2010,30(9):2377-2380.
[11]史训瑶,杨小勇,左闻宇,等.烘箱法及气相色谱法测定烟叶水分及其差异分析[J].广东化工,2015,42(23):193-194.
[12]贾敏鸽,王燕,许丹,等.中药丸剂中水分的GC法测定[J].药物分析杂志,2004,24(6):616-619.
[13]GB/T 23203.1-2013卷烟总粒相物中水分的测定第1部分:气相色谱法[S].
[14]伍锦鸣,彭斌,刘克建,等.气相色谱法测定烟草含水率[J].烟草科技,2012(12):49-51.
[15]YC/T 345-2010烟草及烟草制品水分的测定气相色谱法[S].
[16]GB/T 6682-2008分析实验室用水规格和试验方法[S].