气相色谱-质谱法测定苦苣菜、葡萄籽超临界萃取物中的脂肪酸含量
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摘要
通过气相色谱-质谱联用仪对苦苣菜、葡萄籽的CO_2超临界萃取物进行成分分析,得到主要成分为脂肪酸类,对其脂肪酸建立定性定量方法,以准确分析其萃取物的脂肪酸含量。运用优化的CO_2超临界萃取方法得到苦苣菜、葡萄籽提取物,通过气质联用仪及NIST谱库对提取物进行成分分析,改进气相色谱条件(色谱柱为HP-5msUI,分析时间为57min),优化质谱条件(单反应监测模式和分段扫描),得到多种脂肪酸的定性定量方法。通过气质联用仪解析了苦苣菜CO_2超临界提取物的活性成分,脂肪酸测定方法对于植物提取物具有较好的线性关系(相关系数R均高于0.992 0)、回收率在80%～105%之间,定量限在0.002～0.010 g/kg之间,RSD均小于4.0%。测得苦苣菜萃取物中有20种脂肪酸,不饱和脂肪酸占总脂肪酸的83.5%,葡萄籽萃取物中检出了10种脂肪酸,不饱和脂肪酸占总脂肪酸的91.74%。脂肪酸测定方法操作简便、灵敏度高,缩短了检验时间,适用于植物萃取物中脂肪酸的测定。解析了苦苣菜的活性成分,得到了苦苣菜、葡萄籽中脂肪酸的准确含量。
A method for the determination of fatty acids by gas chromatography-mass spectrometry was established to analyze the fatty acids in the supercritical CO_2 extracts of Sonchus oleraceus L. and grape seeds. By using the improved gas chromatography conditions(HP-5 msUI column was adopted and analysis time was 57 min.), the optimized mass spectrometry conditions(selected ion monitoring mode and segment detection) were used to analyze the types and contents of fatty acids of supercritical CO_2 extracts of Sonchus oleraceus L. and grape seeds. This method had a good linear relationship, the correlation coefficient(R)was above 0.992 0, the recoveries were within80%～105%, the RSD of precision was less than 4.0%,the quantitative limit was between 0.002 and 0.010 g/kg. It was found that there were 20 kinds of fatty acids in that extract of the Sonchus oleraceus L., the unsaturated fatty acid accounted for 83.5% of the total fatty acid, 10 kinds of fatty acids were detected in the grape seed extract, and the unsaturated fatty acid accounted for 91.74% of the total fatty acid. The method is simple and sensitive, and it can reduce the cost of testing, shorten the testing time. It is applicable to the determination of fatty acids in plant extracts.
A method for the determination of fatty acids by gas chromatography-mass spectrometry was established to analyze the fatty acids in the supercritical CO_2 extracts of Sonchus oleraceus L. and grape seeds. By using the improved gas chromatography conditions(HP-5 msUI column was adopted and analysis time was 57 min.), the optimized mass spectrometry conditions(selected ion monitoring mode and segment detection) were used to analyze the types and contents of fatty acids of supercritical CO_2 extracts of Sonchus oleraceus L. and grape seeds. This method had a good linear relationship, the correlation coefficient(R)was above 0.992 0, the recoveries were within80%～105%, the RSD of precision was less than 4.0%,the quantitative limit was between 0.002 and 0.010 g/kg. It was found that there were 20 kinds of fatty acids in that extract of the Sonchus oleraceus L., the unsaturated fatty acid accounted for 83.5% of the total fatty acid, 10 kinds of fatty acids were detected in the grape seed extract, and the unsaturated fatty acid accounted for 91.74% of the total fatty acid. The method is simple and sensitive, and it can reduce the cost of testing, shorten the testing time. It is applicable to the determination of fatty acids in plant extracts.
引文
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[11]刘明,魏芳,谢亚,等.基于衍生化技术的游离脂肪酸的色谱-质谱分析方法研究进展[J].分析测试学报,2017,36(10):1269-1278.
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[14]张红英,姚元虎,颜雪明.超临界流体萃取分离技术及其应用[J].首都师范大学学报:自然科学版,2016,37(6):50-53.
[2]崔文燕,刘素香,宋晓凯等.黄花败酱草和白花败酱草的化学成分与药理作用研究进展[J].药物评价与研究,2016,39(3):482-488.
[3]Ting Huyan,Qi Li,Yi-Lin Wang,et al.Anti-tumor effect of hot aqueous extracts from Sonchus oleraceus(L.)L.and Juniperus sabina L-Two traditional medicinal plants in China[J].Journal of Ethnopharmacology,2016,185:289-299.
[4]O.Kenny,T.J.Smyth,D.Walsh,et al.Investigating the potential of under-utilised plants from the Asteraceae family as a source of natural antimicrobial and antioxidant extracts[J].Food Chemistry,2014,161:79-86.
[5]Mohamed ZM Salem,Hayssam M Ali,Nader A El-Shanhorey,et al.Evaluation of extracts and essential oil from Callistemon viminalis leaves:Antibacterial and antioxidant activities,total phenolic and flavonoid contents[J].Asian Pacific Journal of Tropical Medicine,2013,6(10):785-791.
[6]王金兰,王丹,李军,等.中华苦荬菜中的新三萜[J].中草药,2015,46(22):3304-3309.
[7]Kyung-su Kima,Won-Gul Hwang,Hong-Gi Jang,et al.Assessment of Indigo(Polygonum tinctorium Ait.)water extracts’bioactive compounds,and their antioxidant and antiproliferative activities[J].LWT-Food Science and Technology,2012,46(2):500-510.
[8]王丽娟,杨宋琪,郭兴霞,等.响应面法优化超声波辅助提取葡萄籽中油脂及其脂肪酸成分分析[J].粮食与油脂,2018,31(3):49-51.
[9]魏玲玲,陈竞男,王杰.葡萄籽中油脂脂肪酸和蛋白质组分分析[J].粮食与油脂,2017,30(12):65-68.
[10]田翔,乔治军,田琴,等.气相色谱-质谱法定性定量测定糜子中的脂肪酸[J].食品科学,2016,37(14):128-131.
[11]刘明,魏芳,谢亚,等.基于衍生化技术的游离脂肪酸的色谱-质谱分析方法研究进展[J].分析测试学报,2017,36(10):1269-1278.
[12]中华人民共和国卫生部.GB 5009.168-2016食品中脂肪酸的测定[S].北京:中国标准出版社,2016.
[13]瞿研,贺成,张建军,等.超临界CO2萃取阿萨伊油的工艺优化及GC-MS分析[J].食品工业科技,2018,39(9):257-261.
[14]张红英,姚元虎,颜雪明.超临界流体萃取分离技术及其应用[J].首都师范大学学报:自然科学版,2016,37(6):50-53.