快速溶剂萃取GC-MS分析不同枣的挥发性成分
|
摘要
目的:建立枣中挥发性成分分析方法,鉴定其化学成分。方法:采用快速溶剂萃取(ASE)-气质联用(GC-MS)法分析不同枣中挥发性成分,利用峰面积归一化法测定各成分的相对百分含量。比较ASE和索式提取(SE)2种提取方法对大枣枣果中挥发性成分提取效果的差异,同时考察ASE法下不同溶剂(80%乙醇和石油醚)对挥发性成分提取效率的影响,探讨了提取物甲酯化处理后对提取挥发性成分的影响,并利用主成分分析比较了9种枣中挥发性成分的差异。结果:ASE法以80%乙醇为提取剂较为高效、安全。对河北行唐大枣甲酯化处理后发现更多的挥发性成分,比未甲酯化处理多18种成分。9种枣果中不饱和脂肪酸相对含量占45.3%~70.3%,其中十六烯酸(甲酯)相对含量最高,可达24.0%~38.3%。将9种枣果18个共有峰相对含量采用主成分分析评价不同产地的枣果品质,9种枣果得到有效区分,其中武邑马牙枣品质最佳,其次为武邑小枣、香河小枣和武邑大枣。结论:不同地区、不同品种枣果挥发性成分存在一定的差异性。该实验可为开发枣资源提供参考依据。
Objective: To analyze the volatile components in Jujubae Fructus and identify the chemical compositions. Method: An accelerated solvent extraction(ASE) gas chromatography-mass spectrometry(GCMS) method was applied for the analysis of volatile components in Jujubae Fructus. The relative percentage contents of the volatile components were determined by the peak area normalization method. Based on the extraction efficiency,two extraction methods including ASE and soxhlet extraction(SE) were investigated and compared for the extraction of volatile components,and the effects of two different solvents(80% ethanol and petroleum ether)were also investigated under the ASE method. In addition,the difference between the volatile components of the extracts before and after methyl esterification treatment was investigated,and the volatile components of the extracts from 9 kinds of Jujubae Fructus were compared by using principal component analysis. Result: The results showed that ASE method with 80% ethanol as the extract solvent was more efficient and safer. More 18 volatile components could be found after methyl esterification treatment in the extract of Hebei Xingtang Jujubae Fructus. The relative contents of unsaturated fatty acids in 9 kinds of Jujubae Fructus were up to 45. 3%-70. 3%,of which the relative content of hexadecenoic acid(methyl ester) was the highest and up to 24. 0%-38. 3%. Principal component analysis was applied for evaluation of the qualities through the common 18 volatile components in the extracts of 9 Jujubae Fructus samples from different regions. In this way,these 9 Jujubae Fructus samples from different regions were effectively distinguished and it was indicated that the best Jujubae Fructus was from Wuyi Mayazao,followed by Wuyi Xiaozao, Xianghe Xiaozao and Wuyi Dazao. Conclusion: There are certain differences in volatile components of Jujubae Fructus from different regions and varieties. This experiment can provide references for the development of jujube resources.
Objective: To analyze the volatile components in Jujubae Fructus and identify the chemical compositions. Method: An accelerated solvent extraction(ASE) gas chromatography-mass spectrometry(GCMS) method was applied for the analysis of volatile components in Jujubae Fructus. The relative percentage contents of the volatile components were determined by the peak area normalization method. Based on the extraction efficiency,two extraction methods including ASE and soxhlet extraction(SE) were investigated and compared for the extraction of volatile components,and the effects of two different solvents(80% ethanol and petroleum ether)were also investigated under the ASE method. In addition,the difference between the volatile components of the extracts before and after methyl esterification treatment was investigated,and the volatile components of the extracts from 9 kinds of Jujubae Fructus were compared by using principal component analysis. Result: The results showed that ASE method with 80% ethanol as the extract solvent was more efficient and safer. More 18 volatile components could be found after methyl esterification treatment in the extract of Hebei Xingtang Jujubae Fructus. The relative contents of unsaturated fatty acids in 9 kinds of Jujubae Fructus were up to 45. 3%-70. 3%,of which the relative content of hexadecenoic acid(methyl ester) was the highest and up to 24. 0%-38. 3%. Principal component analysis was applied for evaluation of the qualities through the common 18 volatile components in the extracts of 9 Jujubae Fructus samples from different regions. In this way,these 9 Jujubae Fructus samples from different regions were effectively distinguished and it was indicated that the best Jujubae Fructus was from Wuyi Mayazao,followed by Wuyi Xiaozao, Xianghe Xiaozao and Wuyi Dazao. Conclusion: There are certain differences in volatile components of Jujubae Fructus from different regions and varieties. This experiment can provide references for the development of jujube resources.
引文
[1]刘世军,唐志书,崔春利,等.大枣化学成分的研究进展[J].云南中医学院学报,2015,38(3):96-100.
[2]王蓉珍,赵子青,林勤保,等.大枣功效成分检测的研究进展[J].食品工业科技,2012,33(4):423-426.
[3]刘莎莎,张宝善,孙肖园,等.红枣香味物质的主成分分析[J].食品工业科技,2015,36(20):72-76.
[4]曾立,向荣,尹文清,等.瑶药定心藤挥发油的提取工艺及其GC-MS分析[J].中成药,2012,34(8):1613-1615.
[5]叶丽华,张玮,张丽娟,等.川芎挥发油提取工艺的研究进展[J].药学服务与研究,2012,12(3):195-198.
[6]Rodrigo Scopel,Caroline Finkler da Silva,Aline Machado Lucas,et al.Fluid phase equilibria and mass transfer studies applied to supercritical fluid extraction of Illicium verum volatile oil[J].Fluid Phase Equilibria,2016,417:203-211.
[7]郝红梅,张生万,郭彩霞,等.顶空固相微萃取-气相色谱-质谱联用法分析山楂果醋易挥发成分[J].食品科学,2016,37(2):138-141.
[8]申利群,雷福厚.顶空固相微萃取-气相色谱/质谱法分析霸王花挥发性成分[J].食品科学,2010,31(22):315-317.
[9]Mphahlele R R,Fawole O A,Mokwena L M,et al.Effect of extraction method on chemical,volatile composition and antioxidant properties of pomegranate juice[J].South Afr J Bot,2016(103):135-144.
[10]赵一帆,张东,杨立新,等.HS-SPME-GC-MS测定洋甘菊不同部位挥发性成分[J].中国实验方剂学杂志,2018,24(2):69-73.
[11]GUO Q,GAO S,SUN Y W,et al.Antioxidant efficacy of rosemary ethanol extract in palm oil during frying and accelerated storage[J].Ind Crop Prod,2016(94):82-88.
[12]刘慧,姚蓝,陈建红,等.栀子不同炮制品中挥发油类成分的GC-MS分析[J].中国中药杂志,2015,40(9):1732-1737.
[13]郑勇凤,汪蕾,赵思蕾,等.应用自动质谱退卷积定性系统(AMDIS)和保留指数分析3种不同基原莪术的挥发油成分差异[J].中国中药杂志,2016,41(2):257-263.
[14]薛鹏,杨立新,曹英夕,等.水蒸气蒸馏及不同萃取纤维对白花蛇舌草挥发性成分分析[J].中国实验方剂学杂志,2017,23(6):85-90.
[15]甘彦雄,罗妮妮,蒋燕萍,等.基于GC-MS同时测定蓬莪术及其醋制品挥发油中β-榄香烯、莪术醇、吉马酮、新莪术二酮的含量[J].中国中药杂志,2015,40(7):1311-1315.
[16]宋丽,郑明珠,王立江.响应面法优化长白山野菊花挥发油的提取工艺及成分分析[J].食品与发酵工业,2016,42(7):181-187.
[17]王媚,史亚军,郭东艳,等.延胡索挥发油的红外光谱法与气相色谱-质谱分析[J].中南药学,2017,15(1):99-102.
[18]郭鹏,李琳琳,刘翔.中草药川楝子挥发油与微量元素的成分分析[J].大连民族大学学报,2017,19(3):212-215.
[19]朱凤妹,李军,高海生,等.金丝小枣与山西大枣中芳香性成分的研究[J].中国食品添加剂,2010(3):119-124.
[20]开赛尔·买买提明·特肯,苏豫梅,杜辉辉,等.新疆尖果沙枣中生物挥发油组分的鉴定及脂肪酸含量的测定[J].农产品加工:学刊,2014(3):75-76,78.
[21]张合川,徐如彦.大枣挥发油的提取分析及其在烟草中应用研究[J].轻工科技,2013,29(12):17-18.
[22]陆钊,高凯,潘淑霞,等.加速溶剂萃取/气相色谱-质谱法分析朝鲜淫羊藿挥发油成分[J].哈尔滨工业大学学报,2011,43(8):145-148.
[23]杨璐,李承隆,肖华林,等.海南江蓠挥发油化学成分的研究[J].化学与生物工程,2015,32(1):64-66.
[24]姚广龙,张莉娜,王新广,等.海南大歧舌苔挥发油化学成分的研究[J].化学与生物工程,2016,33(3):59-62.
[25]JIA L H,LIU Y,LI Y Z.Rapid determination of volatile constituents in safflower from Xinjiang and Henan by ultrasonic-assisted solvent extraction and GC-MS[J].J Pharmaceut Anal,2011,1(3):213-218.
[26]Hamid Mellouk,Alice Meullemiestre,Zoulikha MaacheRezzoug,et al.Valorization of industrial wastes from French maritime pine bark by solvent free microwave extraction of volatiles[J].J Cleaner Prod,2016(112):4398-4405.
[27]Kostic'A,Trifunovic'B D,Pe2ic'M B,et al.Fatty acids of maize pollen-quantification,nutritional and morphological evaluation[J].J Cereal Sci,2017,77:180-185.
[28]田光晶,马丛丛,陈萌,等.亚麻籽油抗动脉粥样硬化作用的研究进展[J].中国油脂,2017(10):87-92.
[29]梁欢,卢金清,戴艺,等.HS-SPME-GC-MS结合化学计量法对不同产地艾叶药材挥发性成分的比较分析[J].中国实验方剂学杂志,2014,20(18):85-90.
[2]王蓉珍,赵子青,林勤保,等.大枣功效成分检测的研究进展[J].食品工业科技,2012,33(4):423-426.
[3]刘莎莎,张宝善,孙肖园,等.红枣香味物质的主成分分析[J].食品工业科技,2015,36(20):72-76.
[4]曾立,向荣,尹文清,等.瑶药定心藤挥发油的提取工艺及其GC-MS分析[J].中成药,2012,34(8):1613-1615.
[5]叶丽华,张玮,张丽娟,等.川芎挥发油提取工艺的研究进展[J].药学服务与研究,2012,12(3):195-198.
[6]Rodrigo Scopel,Caroline Finkler da Silva,Aline Machado Lucas,et al.Fluid phase equilibria and mass transfer studies applied to supercritical fluid extraction of Illicium verum volatile oil[J].Fluid Phase Equilibria,2016,417:203-211.
[7]郝红梅,张生万,郭彩霞,等.顶空固相微萃取-气相色谱-质谱联用法分析山楂果醋易挥发成分[J].食品科学,2016,37(2):138-141.
[8]申利群,雷福厚.顶空固相微萃取-气相色谱/质谱法分析霸王花挥发性成分[J].食品科学,2010,31(22):315-317.
[9]Mphahlele R R,Fawole O A,Mokwena L M,et al.Effect of extraction method on chemical,volatile composition and antioxidant properties of pomegranate juice[J].South Afr J Bot,2016(103):135-144.
[10]赵一帆,张东,杨立新,等.HS-SPME-GC-MS测定洋甘菊不同部位挥发性成分[J].中国实验方剂学杂志,2018,24(2):69-73.
[11]GUO Q,GAO S,SUN Y W,et al.Antioxidant efficacy of rosemary ethanol extract in palm oil during frying and accelerated storage[J].Ind Crop Prod,2016(94):82-88.
[12]刘慧,姚蓝,陈建红,等.栀子不同炮制品中挥发油类成分的GC-MS分析[J].中国中药杂志,2015,40(9):1732-1737.
[13]郑勇凤,汪蕾,赵思蕾,等.应用自动质谱退卷积定性系统(AMDIS)和保留指数分析3种不同基原莪术的挥发油成分差异[J].中国中药杂志,2016,41(2):257-263.
[14]薛鹏,杨立新,曹英夕,等.水蒸气蒸馏及不同萃取纤维对白花蛇舌草挥发性成分分析[J].中国实验方剂学杂志,2017,23(6):85-90.
[15]甘彦雄,罗妮妮,蒋燕萍,等.基于GC-MS同时测定蓬莪术及其醋制品挥发油中β-榄香烯、莪术醇、吉马酮、新莪术二酮的含量[J].中国中药杂志,2015,40(7):1311-1315.
[16]宋丽,郑明珠,王立江.响应面法优化长白山野菊花挥发油的提取工艺及成分分析[J].食品与发酵工业,2016,42(7):181-187.
[17]王媚,史亚军,郭东艳,等.延胡索挥发油的红外光谱法与气相色谱-质谱分析[J].中南药学,2017,15(1):99-102.
[18]郭鹏,李琳琳,刘翔.中草药川楝子挥发油与微量元素的成分分析[J].大连民族大学学报,2017,19(3):212-215.
[19]朱凤妹,李军,高海生,等.金丝小枣与山西大枣中芳香性成分的研究[J].中国食品添加剂,2010(3):119-124.
[20]开赛尔·买买提明·特肯,苏豫梅,杜辉辉,等.新疆尖果沙枣中生物挥发油组分的鉴定及脂肪酸含量的测定[J].农产品加工:学刊,2014(3):75-76,78.
[21]张合川,徐如彦.大枣挥发油的提取分析及其在烟草中应用研究[J].轻工科技,2013,29(12):17-18.
[22]陆钊,高凯,潘淑霞,等.加速溶剂萃取/气相色谱-质谱法分析朝鲜淫羊藿挥发油成分[J].哈尔滨工业大学学报,2011,43(8):145-148.
[23]杨璐,李承隆,肖华林,等.海南江蓠挥发油化学成分的研究[J].化学与生物工程,2015,32(1):64-66.
[24]姚广龙,张莉娜,王新广,等.海南大歧舌苔挥发油化学成分的研究[J].化学与生物工程,2016,33(3):59-62.
[25]JIA L H,LIU Y,LI Y Z.Rapid determination of volatile constituents in safflower from Xinjiang and Henan by ultrasonic-assisted solvent extraction and GC-MS[J].J Pharmaceut Anal,2011,1(3):213-218.
[26]Hamid Mellouk,Alice Meullemiestre,Zoulikha MaacheRezzoug,et al.Valorization of industrial wastes from French maritime pine bark by solvent free microwave extraction of volatiles[J].J Cleaner Prod,2016(112):4398-4405.
[27]Kostic'A,Trifunovic'B D,Pe2ic'M B,et al.Fatty acids of maize pollen-quantification,nutritional and morphological evaluation[J].J Cereal Sci,2017,77:180-185.
[28]田光晶,马丛丛,陈萌,等.亚麻籽油抗动脉粥样硬化作用的研究进展[J].中国油脂,2017(10):87-92.
[29]梁欢,卢金清,戴艺,等.HS-SPME-GC-MS结合化学计量法对不同产地艾叶药材挥发性成分的比较分析[J].中国实验方剂学杂志,2014,20(18):85-90.