正交试验优化烟草中高级脂肪酸的皂化条件及UPLC/ELSD分析  

Optimization of Saponification Conditions on High Fatty Acids in Tobacco with Orthogonal Experiments and Their Determination by UPLC/ELSD

作　　者：韩敬美 翟婷[2] 王昆淼[1] 刘春波[1] 何沛[1] 赵伟[1] 刘志华[1] 

机构地区：[1]云南烟草科学研究院云南省烟草化学重点实验室,云南昆明650106 [2]昆明学院化学科学与技术系,云南昆明650214

出　　处：《分析测试学报》2012年第10期1309-1313,共5页Journal of Instrumental Analysis

基　　金：中国烟草总公司科技重大专项项目(110201001001);云南中烟工业公司科技开发计划(2010JC04);云南省创新团队建设项目(2009CI014)

摘　　要：建立了超高效液相色谱/蒸发光散射检测器(UPLC/ELSD)测定烟草中6种高级脂肪酸的方法,其最佳条件为:Waters UPLC BEH C18柱,乙腈-乙酸水溶液(体积比80∶20)梯度洗脱,流速0.3 mL/min,漂移管温度为50℃,气体流速为2.89 L/min。对温度、时间、pH值、萃取剂体积等影响因素进行了研究,并通过正交试验系统地分析了各因素的影响,获得了最佳皂化条件,即:皂化温度60℃,氢氧化钾浓度3 mol/L,二氯甲烷15 mL,反应时间为60 min。方法的线性范围为42.4～520.0 mg/L,检出限为3.64～11.98 mg/L,相对标准偏差为4.9%～13.5%,烟草样品的回收率为83%～104%。In this paper, some high fatty acids in tobacco were analyzed by liquid chromatography with evaporative light-scatter detector （UPLC/ELSD）. fluence factors of the high fatty acids, including temperature, reaction time, tration（pH）, volume of extracting agents, etc, were systematically studied Ultra-high performance The saponification inhydrogen ion concenthrough the orthogonal experiments. The best saponification conditions were as follows： saponification temperature： 60 °C, KOH： 3 mol/L, CH2C12：15 mL, reaction time： 60 min. In addition, a new UPLC/ELSD method was established for the determination of six high fatty acids, including linolenic acid, linoleic acid, palm acid, oleic acid, myristic acid and stearic acid in tobacco on the C1s chromatography column by gradient elution with acetonitrile -acetic acid aqueous solution （80 ： 20, by volume） as mobile phase at a flow rate of 0. 3 mL/min, a drift tube temperature of 50°C and a gas flow rate of 2. 89 L/min. The linear range of the method was in the range of 42. 4 -520. 0 mg/L, with detection limits of 3.64 - 11.98 mg/L. The RSDs（n =7） were in the range of 4. 9% - 13.5% , and the recoverles ranged from 83% to 104%. This method is rapid, convenient and sensitive, and is suitable for the determination of high fatty acids in tobacco.

关 键 词：正交试验 超高效液相色谱 蒸发光散射 烟草 高级脂肪酸 

分 类 号：O657.63[理学—分析化学] TS411[理学—化学]