HS-SPME-GC-MS结合自动解卷积技术分析阿胶中的挥发性成分
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摘要
建立了顶空固相微萃取—气相色谱—质谱(headspace solid phase microextraction-gas chromatography-mass spectrometry,HS-SPME-GC-MS)结合自动解卷积技术检测阿胶中挥发性物质的分析方法。以总峰面积和总出峰数为考察指标,通过单因素和正交试验对萃取条件进行优化,以期得到HS-SPME-GC-MS分析阿胶挥发性物质的较优条件。结果显示,萃取温度对总出峰数和总峰面积的影响较大,所得优化萃取条件为样品量5g、50/30μm DVB/CAR/PDMS萃取头、萃取温度70℃、平衡时间10 min、萃取时间50 min、解吸时间5min。该条件下,鉴定出阿胶挥发性成分41种,分别为吡嗪类10种、醛类8种、酯类5种、酮类6种、13种其他类化合物,其中相对含量较高的为吡嗪类48.95%和醛类26.37%。挥发性成分绝对峰面积的相对标准偏差的平均值为6.25%,该方法重复性较好。
A method for the determination of volatile compounds fromColla Corii Asini by headspace solid-phase microextraction(HS-SPME)coupled with gas chromatography-mass spectrometry(GC-MS)combined with AMDIS was established.The total peak area and number of peaks of the volatile compounds were used as indices to optimize the different extraction conditions by single factor and orthogonal test.The results showed that the influence of extraction temperature was larger. The better extraction conditions were:the sample amount of 5 g,equilibration time 10 min,extracted for 50 min at 70 ℃ by 50/30μm DVB/CAR/PDMS fiber and then desorbed 5 min.Under these conditions,41 species of volatile components from Colla Corii Asini were identified,including 10 pyrazines,8 aldehydes,5 esters,6 ketones and 13 others.Among of these,the higher relative contents were pyrazines and aldehydes,accounting for48.95% and 26.37% of the total components,respectively.The average RSD of the peak area of volatile compounds was 6.25%,which showed that the repeatability of the method was well.This method provides a theoretical basis for the quality control and product research and development of Colla Corii Asini.
A method for the determination of volatile compounds fromColla Corii Asini by headspace solid-phase microextraction(HS-SPME)coupled with gas chromatography-mass spectrometry(GC-MS)combined with AMDIS was established.The total peak area and number of peaks of the volatile compounds were used as indices to optimize the different extraction conditions by single factor and orthogonal test.The results showed that the influence of extraction temperature was larger. The better extraction conditions were:the sample amount of 5 g,equilibration time 10 min,extracted for 50 min at 70 ℃ by 50/30μm DVB/CAR/PDMS fiber and then desorbed 5 min.Under these conditions,41 species of volatile components from Colla Corii Asini were identified,including 10 pyrazines,8 aldehydes,5 esters,6 ketones and 13 others.Among of these,the higher relative contents were pyrazines and aldehydes,accounting for48.95% and 26.37% of the total components,respectively.The average RSD of the peak area of volatile compounds was 6.25%,which showed that the repeatability of the method was well.This method provides a theoretical basis for the quality control and product research and development of Colla Corii Asini.
引文
[1]吴海燕,孙佳明,张辉.阿胶的研究进展[J].吉林中医药,2016,36(1):57-60.
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[12]任恒鑫,张舒婷,吴宏斌,等.GC-MS-AMDIS结合保留指数分析藿香挥发油[J].食品科学,2013,34(24):230-232.
[13]何志海,侯功坦,梁虹瑜,等.气相色谱质谱联用法分析藿香正气口服液中的挥发性成分[J].分析试验室,2014,33(2):229-235.
[14]YAN Jun,LIU Xin-bo,ZHU Wei-wei,et al.Retention Indices for Identification of Aroma Compounds by GC:Development and Application of a Retention Index Database[J].Chromatographia,2015,78(1):89-108.
[15]EZQUERRO,PONS B,TENA M T.Development of a headspace solid-phase microextraction-gas chromatographymass spectrometry method for the identification of odourcausing volatile compounds in packaging materials[J].Journal of Chromatography A,2002,963(1):381-392.
[16]魏长庆,周琦,刘文玉.HS-SPME-GC-MS分析新疆胡麻油挥发性成分的技术优化[J].食品科学,2017,38(14):151-157.
[17]艾对,张富新,于玲玲,等.羊奶中挥发性成分顶空固相微萃取条件的优化[J].食品与生物技术学报,2015,34(1):40-46.
[18]薛妍君,张丽,冯莉,等.荠菜芳香成分的固相微萃取条件优化与分析[J].食品工业科技,2015,36(1):328-333.
[19]王双.利用全二维气质联用仪对剑南春白酒中吡嗪类生理活性物质的研究[J].酿酒,2016,43(5):49-50.
[20]孙惜时,李文华,李荣,等.芝麻香型白酒中硫化物和吡嗪类成分的抗氧化活性[J].酿酒,2013,40(4):57-60.
[2]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:190.
[3]MA L X,AI P,LI H,et al.The prophylactic use of Chinese herbal medicine for chemotherapy-induced leucopenia in oncology patients:a systematic review and meta-analysis of randomized clinical trials[J].Support Care Cancer,2015,23(2):561-579.
[4]LIU Mao-xuan,TAN Hai-ning,ZHANG Xin-ke,et al.Hematopoietic effects and mechanisms of Fufang ejiao jiang on radiotherapy and chemotherapy-induced myelosuppressed mice[J].Journal of Ethnopharmacology,2014,152(3):575-584.
[5]WANG Dong-liang,LIU Mao-xuan,CAO Ji-chao,et al.Effect of Colla corii asini(Ejiao)on D-galactose induced aging mice[J].Biological and Pharmaceutical Bulletin,2012,35(12):2 128-2 132.
[6]付玥,张茹,吴昊轩,等.阿胶的研究进展[J].新经济,2014(8):18-19.
[7]张晶,朱建才,曾俊,等.阿胶产品的香气分析与风味调控[J].上海应用技术学院学报:自然科学版,2014,14(4):295-298.
[8]毛跟年,郭倩,李鑫,等.气相色谱-质谱联用法分析阿胶中的腥味物质[J].动物医学进展,2010,31(12):72-75.
[9]王进,朱建才.应用GC-MS/GC-O法鉴定阿胶关键香气化合物[J].食品工业,2016,37(7):265-269.
[10]佘远斌,舒畅,肖作兵,等.GC-MS/GC-O结合化学计量学方法研究不同产地阿胶的关键香气组分[J].现代食品科技,2016,32(2):269-275.
[11]肖作兵,舒畅,牛云蔚,等.不同产地阿胶的挥发性成分分析[C]//第十届中国香料香精学术研讨会论文集.北京:中国香料香精化妆品工业协会,2014:161-166.
[12]任恒鑫,张舒婷,吴宏斌,等.GC-MS-AMDIS结合保留指数分析藿香挥发油[J].食品科学,2013,34(24):230-232.
[13]何志海,侯功坦,梁虹瑜,等.气相色谱质谱联用法分析藿香正气口服液中的挥发性成分[J].分析试验室,2014,33(2):229-235.
[14]YAN Jun,LIU Xin-bo,ZHU Wei-wei,et al.Retention Indices for Identification of Aroma Compounds by GC:Development and Application of a Retention Index Database[J].Chromatographia,2015,78(1):89-108.
[15]EZQUERRO,PONS B,TENA M T.Development of a headspace solid-phase microextraction-gas chromatographymass spectrometry method for the identification of odourcausing volatile compounds in packaging materials[J].Journal of Chromatography A,2002,963(1):381-392.
[16]魏长庆,周琦,刘文玉.HS-SPME-GC-MS分析新疆胡麻油挥发性成分的技术优化[J].食品科学,2017,38(14):151-157.
[17]艾对,张富新,于玲玲,等.羊奶中挥发性成分顶空固相微萃取条件的优化[J].食品与生物技术学报,2015,34(1):40-46.
[18]薛妍君,张丽,冯莉,等.荠菜芳香成分的固相微萃取条件优化与分析[J].食品工业科技,2015,36(1):328-333.
[19]王双.利用全二维气质联用仪对剑南春白酒中吡嗪类生理活性物质的研究[J].酿酒,2016,43(5):49-50.
[20]孙惜时,李文华,李荣,等.芝麻香型白酒中硫化物和吡嗪类成分的抗氧化活性[J].酿酒,2013,40(4):57-60.