由α-氯代酸制备α-癸基甜菜碱产物的全组分分析

doi:10.13218/j.cnki.csdc.2014.03.038

摘要/Abstract

摘要： 针对α-氯代十二酸(CDA)与三甲胺反应制备α-癸基甜菜碱(CB)的工艺路线,采用HPLC-ELSD法分析合成产物中的CB含量,采用索氏抽提法萃取残留脂肪酸,并用气相色谱(GC)进一步分析残留脂肪酸中十二酸(DA)、CDA和α-羟基十二酸(HDA)的相对含量。以V(甲醇)∶V(水)=7∶1的混合溶液为流动相,HPLC-ELSD的峰信号分离度高,在质量浓度0.004～0.08 g·L^-1内线性关系、精密度和准确性较好;以石油醚(60～90 ℃)为萃取溶剂可以将残留脂肪酸萃取完全,结合GC测试,可定量分析DA,CDA和HDA。

关键词: α-癸基甜菜碱, 脂肪酸, 高效液相-蒸发光散射法, 索氏抽提, 气相色谱法

Abstract: α-Capric betaine (CB) was prepared from α-chlorododecanoic acid (CDA) and trimethylamine (TMA) as starting materials.The content of CB in the product was analyzed adopting HPLC-ELSD method.The residual fatty acids containing in the product were extracted with Soxhlet extractor and then the relative content of dodecanoic acid (DA),CDA and α-hydroxydodecanoic acid (HDA) in the residual of fatty acid extract were further analyzed with gas chromatography (GC).Results showed that,using a solution composed of V(methanol)∶V(water)=7∶1 as the mobile phase of HPLC-ELSD,the linear relationship,the reproducibility and the accuracy were good and the signal separation is high in the mass concentration range of 0.004-0.08 g·L^-1;the residual fatty acids can be completely extracted with petroleum ether (60-90 ℃) as the solvent of Soxhlet extraction,and the relative content of DA,CDA and HDA can be quantitatively analyzed using GC.

Key words: α-capric betaine, fatty acid, HPLC-ELSD, Soxhlet extraction, gas chromatography

中图分类号:

TQ423.3

梅杰, 张永民, 刘雪锋, 方云. 由α-氯代酸制备α-癸基甜菜碱产物的全组分分析[J]. 日用化学工业, 2014, 44(3): 167-170.

MEI Jie, ZHANG Yong-min, LIU Xue-feng, FANG Yun. Total component analysis of α-capric betaine product prepared from α-chloro fatty acid[J]. China Surfactant Detergent & Cosmetics, 2014, 44(3): 167-170.

参考文献

[1] LI NA,ZHANG GUICAI,GE JIJIANG,et al.Adsorption behavior of betaine-type surfactant on quartz sand[J].Energy Fuels,2011,25(10):4430-4437.
[2] QUAN HONGPING,ZHANG XUAN,LU HONGSHENG,et al.Synthesis and acid solution properties of a novel betaine zwitterionic surfactant[J].Cent Eur J Chem,2012,10(5):1624-1632.
[3] NIE HONGQIAN,SONG SHUE,HOU WANGGUO.Vesicles formation induced by layered double hydroxides in mixture of lauryl sulfonate betaine and sodium dodecyl benzenesulfonate[J].Chin J Chem,2011,29(7):1373-1379.
[4] WANG ZEYUN,ZHANG SHUFEN,FANG YUN,et al.Synergistic behavior between zwitterionic surfactant α-decylbetaine and anionic surfactant sodium dodecyl sulfate[J].J Surfact Deterg,2010,13(4):381-385.
[5] 夏纪鼎,倪永全.表面活性剂和洗涤剂化学与工艺学[M].北京:中国轻工业出版社,1997:344-345.
[6] 方云.两性表面活性剂[M].北京:中国轻工业出版社,2001:110-113.
[7] 夏咏梅,方云,张明胜.天然油脂基两性表面活性剂的合成和性质Ⅱ:α-氯代长链脂肪酸的合成[J].日用化学工业,1994(3):1-3.
[8] 夏咏梅,方云,何家荣,等.天然油脂基两性表面活性剂的合成和性质Ⅲ:α-长链烷基甜菜碱的合成和性质[J].日用化学工业,1994(4):166-168.
[9] 梁刚.α-长链烷基甜菜碱无溶剂法工艺研究[D].无锡:江南大学,2011.
[10] 张锦阳.α-长链烷基甜菜碱的定量分析[D].无锡:江南大学,2009.
[11] 胡瑜.α-长链烷基-N,N-二甲基甘氨酸的合成与衍生化[D].无锡:江南大学,2012.
[12] AMY L PAYEUR,MATTHEW A LORENZ,ROBERT T KENNEDY.Analysis of fatty acid composition in insulin secreting cells by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry[J].J Chromatogr B,2012,893-894:187-192.
[13] SODAMADE A,OYEDEPO T A,BOLAJI O S.Fatty acids composition of three different vegetable oils (soybean oil,groundnut oil and coconut oil) by high-performance liquid chromatography[J].Chem Mater Res,2013,3(7):26-29.
[14] 钟雷,丁悠丹.表面活性剂及其助剂分析[M].杭州:浙江科学技术出版社,1986:98-101.
[15] 张锦阳,齐丽云,丁宝妹,等.HPLC-ELSD法定量分析α-癸基甜菜碱产品组成[J].中国洗涤用品工业,2009(4):68-70.
[16] 梅杰,刘雪锋,方云,等.溴甲酚绿两相滴定法快速测定α-癸基甜菜碱残留脂肪酸的研究[J].中国洗涤用品工业,2013(8):65-68.
[17] 王美刚.长链脂肪酸α-氯代反应的工艺优化研究[D].无锡:江南大学,2008.
[18] 陈文福.α-羟基脂肪酸的合成及其用于制备α-硫酸化脂肪酸二钠盐[D].无锡:江南大学,2011.