同时蒸馏萃取结合气质联用分析牦牛酥油中特征挥发性物质
|
摘要
采用同时蒸馏萃取结合气质联用分析的方法对牦牛酥油以及其他奶制品中的挥发性风味物质进行提取与分析,从牦牛酥油中共鉴定出65种挥发性物质,与外观、色泽相似的其他奶制品进行对比分析发现,乳酸乙酯、辛酸乙酯、癸酸乙酯是牦牛酥油独特风味中重要的特征挥发性成分。建立这3种物质的内标定量分析方法,线性相关系数R2≥0. 997,线性范围为1. 0～50. 0μg/m L;乳酸乙酯检出限为0. 13μg/kg、回收率在86. 7%～104. 7%;辛酸乙酯检出限为0. 18μg/kg、回收率在89. 3%～98. 4%;癸酸乙酯检出限为0. 17μg/kg、回收率在83. 3%～89. 5%;相对标准偏差RSD值<2. 1%,测定牦牛酥油中乳酸乙酯含量范围在0. 54～5. 14 mg/kg,辛酸乙酯范围在0. 28～2. 20 mg/kg,癸酸乙酯范围在0. 34～3. 84 mg/kg。该方法能有效的去除复杂基质干扰,灵敏度好、准确性高。为区分牦牛酥油与其他相似奶制品、以及评价不同酥油间的风味品质提供了参考方法。
This study extracted and analyzed volatile compounds in yak butter and other similar dairy products by simultaneous distillation extraction combined with GC-MS. There were 65 volatile compounds identified from yak butter,and ethyl lactate,ethyl caprylate,and ethyl caprate were important characteristic volatile compositions. A quantitative analysis method for these three substances was established,and the linear range was 1. 0-50. 0 μg/m L for all with R2≥0. 997. The detection limits of ethyl lactate,ethyl caprylate,and ethyl caprate were 0. 13 μg/kg,0. 18μg/kg,and 0. 17 μg/kg,respectively,and their recovery rates were 86. 7%-104. 7%,89. 3%-98. 4%,and83. 3%-89. 5%,respectively. The RSD of the method was less than 2. 1%. Besides,the measurable ranges of ethyl lactate,ethyl caprylate,and ethyl caprate in yak butter by this method were 0. 54-5. 14 mg/kg,0. 28-2. 20 mg/kg,and 0. 34-3. 84 mg/kg,respectively. The method can effectively eliminate interferences from the complex matrix of yak butter,which resulted its high sensitivity and good accuracy. This study provides a key reference for distinguishing yak butter from other similar dairy products,as well as evaluating the flavor quality of different yak butter.
This study extracted and analyzed volatile compounds in yak butter and other similar dairy products by simultaneous distillation extraction combined with GC-MS. There were 65 volatile compounds identified from yak butter,and ethyl lactate,ethyl caprylate,and ethyl caprate were important characteristic volatile compositions. A quantitative analysis method for these three substances was established,and the linear range was 1. 0-50. 0 μg/m L for all with R2≥0. 997. The detection limits of ethyl lactate,ethyl caprylate,and ethyl caprate were 0. 13 μg/kg,0. 18μg/kg,and 0. 17 μg/kg,respectively,and their recovery rates were 86. 7%-104. 7%,89. 3%-98. 4%,and83. 3%-89. 5%,respectively. The RSD of the method was less than 2. 1%. Besides,the measurable ranges of ethyl lactate,ethyl caprylate,and ethyl caprate in yak butter by this method were 0. 54-5. 14 mg/kg,0. 28-2. 20 mg/kg,and 0. 34-3. 84 mg/kg,respectively. The method can effectively eliminate interferences from the complex matrix of yak butter,which resulted its high sensitivity and good accuracy. This study provides a key reference for distinguishing yak butter from other similar dairy products,as well as evaluating the flavor quality of different yak butter.
引文
[1]白佩君.论酥油(玛尔)的社会文化内涵[J].青海民族研究,2013,24(4):79-82.
[2]杨群.浅谈酥油文化与藏民族精神生活之间的关系[J].新西部,2015(35):38-39.
[3]石燕,郑为完,熊华,等.西藏酥油香气成分的初步分析[J].食品与发酵工业,2006,32(2):90-92.
[4]谭大明,吴雪莲,邱城,等.西藏自治区酥油、糌粑、青稞酒、风干牛肉质量安全调研[J].现代农业科技,2011(2):368-369.
[5]刘晓堂,边巴卓玛,陈红.酥油卫生微生物学评价[J].西藏科技,1994(4):73-74.
[6]喻峰,熊华,吕蓓蕾.西藏牦牛酥油脂肪酸成分分析及功能特性评价[J].中国油脂,2006,31(11):35-38.
[7]周小玲,刘书杰,崔占洪,等.牦牛酥油与普通奶油中脂肪酸组成与含量的比较[J].中国饲料,2008(23):21-23.
[8] NEUPANEY D,KIM J B,ISHIOROSHI M,et al. Study on some functional and compositional properties of yak butter lipid[J]. Animal Science Journal,2003,74(5):391-397.
[9]薛璐,张琦,胡志和.顶空固相微萃取气相色谱质谱法测定内蒙酥油风味物质[J].食品工业科技,2013,34(8):61-64.
[10] HU Songqing,LIU Hai,WEI Shasha,et al. Flavor evaluation of yak butter in Tsinghai-Tibet Plateau and isolation of microorganisms contributing flavor[J]. Animal Science Journal,2011,82(1):122–126.
[11]鲁玉侠,李香莉,卢六美.基于SDE_GC_MS制备的藏酥油香精及其应用[J].现代食品科技,2014,30(2):255-258.
[12]孙美青,马莺,程金菊.牦牛酥油理化性质研究[J].中国乳品工业,2016,44(3):9-11.
[13]安红梅,尹建军,张晓磊.同时蒸馏萃取技术在食品分析中的应用[J].食品研究与开发,2011,12:216-220.
[14] KALUA C M,BEDGOOD D R,PRENZLER P D. Development of a headspace solid phase microextraction-gas chromatography method for monitoring volatile compounds in extended time-course experiments of olive oil[J]. Analytica Chimica Acta,2006,556(2):407-414.
[15]李桂花,何巧红,杨君.一种提取复杂物质中易挥发组分的有效方同时蒸馏萃取及其应用[J].理化检验,2009,4:491-496.
[16]张丽珠,黄湛,唐洁,等,同时蒸馏萃取法和固相微萃取法分析棕榈油与菜籽油复合火锅底料中的风味物质[J].食品科学,2014,35(18):156-160.
[17]张宁,陈海涛,孙宝国,等.固相微萃取和同时蒸馏萃取方法比较传统腊牛肉的风味成分[J].中国食品学报,2016,16(6):247-255.
[18] PINHO O,P R S C,FERREIRA I M P L V O. Solidphase micro extraction of volatile compounds in “Terrincho”ewe cheese comparison of different fibers[J]. Journal of Chromatography A,2003,1011(1-2):1-9.
[19]衣宇佳,田怀香,郑小平,等.同时蒸馏萃取和固相微萃取法提取国产干酪中风味物质[J].食品与机械,2008,24(2):65-69.
[20]李丽梅,郑振山,何近刚,等.不同品种梨酒挥发性成分的SPME-GC-MS结果比较[J].食品工业科技,2016,11:314-331.
[21]马艳丽,曹雁平,杨贞耐,等. SPME-GC-MS检测不同中西方奶酪的挥发性风味物质及比较[J].食品科学,2013,34(20):103-107.
[22] LI Xiujuan,YE Changwen,HUO Xuelian. Solid-phasemicroextraction using adiglycidyloxycalix
[4]arene coated fiber combined with gas chromatography:Very simple,rapid and sensitive method for the determination of chlorobenzenes in water[J]. MicrochimActa,2010,168:161-167.
[23] STASHENKO E E,MARTíNEZ J R. Sampling volatile compounds from natural products with headspace/solidphase micro-extraction[J]. Journal of Biochemical&Biophysical Methods,2007,70(2):235-242.
[24]孙宝国.食用调香术[M].北京:化学工业出版社,2003:475-494.
[25]栾金水.黄酒中风味物质的研究[J].中国酿造,2002,6:21-24.
[26]邹建凯.气相色谱/质谱研究中国干红葡萄酒香味成分[J].分析化学,2001(4):493-493.
[27] RIU-AUMATELL M,MIRP,SERRA-CAYUELA A,et al. Assessment of the aroma profiles of low-alcohol beers using HS-SPME–GC-MS[J]. Food Research International,2014,57(1):196-202.
[28]张防宇.反相高效液相色谱法测定白酒中乙酸乙酯和苯乙醇的含量[J].酿酒科技,2008,11:108-111.
[29] JUN Hyun-Il,YANG Jae-heon,CHOI Ji-yeon. Changes in volatile flavor compounds in steam-dried Allium hookeriroot[J]. Food Science and Biotechnology,2016,25(5):1 327-1 331.
[30]次顿,达珍,白玛玉珍,等.西藏糌粑主要理化指标及质量现状研究[J].西藏科技,2011(3):18-21.
[31]张琦,薛璐,胡志和.传统酥油研究进展[J].食品工业科技,2013,34(8):361-364.
[2]杨群.浅谈酥油文化与藏民族精神生活之间的关系[J].新西部,2015(35):38-39.
[3]石燕,郑为完,熊华,等.西藏酥油香气成分的初步分析[J].食品与发酵工业,2006,32(2):90-92.
[4]谭大明,吴雪莲,邱城,等.西藏自治区酥油、糌粑、青稞酒、风干牛肉质量安全调研[J].现代农业科技,2011(2):368-369.
[5]刘晓堂,边巴卓玛,陈红.酥油卫生微生物学评价[J].西藏科技,1994(4):73-74.
[6]喻峰,熊华,吕蓓蕾.西藏牦牛酥油脂肪酸成分分析及功能特性评价[J].中国油脂,2006,31(11):35-38.
[7]周小玲,刘书杰,崔占洪,等.牦牛酥油与普通奶油中脂肪酸组成与含量的比较[J].中国饲料,2008(23):21-23.
[8] NEUPANEY D,KIM J B,ISHIOROSHI M,et al. Study on some functional and compositional properties of yak butter lipid[J]. Animal Science Journal,2003,74(5):391-397.
[9]薛璐,张琦,胡志和.顶空固相微萃取气相色谱质谱法测定内蒙酥油风味物质[J].食品工业科技,2013,34(8):61-64.
[10] HU Songqing,LIU Hai,WEI Shasha,et al. Flavor evaluation of yak butter in Tsinghai-Tibet Plateau and isolation of microorganisms contributing flavor[J]. Animal Science Journal,2011,82(1):122–126.
[11]鲁玉侠,李香莉,卢六美.基于SDE_GC_MS制备的藏酥油香精及其应用[J].现代食品科技,2014,30(2):255-258.
[12]孙美青,马莺,程金菊.牦牛酥油理化性质研究[J].中国乳品工业,2016,44(3):9-11.
[13]安红梅,尹建军,张晓磊.同时蒸馏萃取技术在食品分析中的应用[J].食品研究与开发,2011,12:216-220.
[14] KALUA C M,BEDGOOD D R,PRENZLER P D. Development of a headspace solid phase microextraction-gas chromatography method for monitoring volatile compounds in extended time-course experiments of olive oil[J]. Analytica Chimica Acta,2006,556(2):407-414.
[15]李桂花,何巧红,杨君.一种提取复杂物质中易挥发组分的有效方同时蒸馏萃取及其应用[J].理化检验,2009,4:491-496.
[16]张丽珠,黄湛,唐洁,等,同时蒸馏萃取法和固相微萃取法分析棕榈油与菜籽油复合火锅底料中的风味物质[J].食品科学,2014,35(18):156-160.
[17]张宁,陈海涛,孙宝国,等.固相微萃取和同时蒸馏萃取方法比较传统腊牛肉的风味成分[J].中国食品学报,2016,16(6):247-255.
[18] PINHO O,P R S C,FERREIRA I M P L V O. Solidphase micro extraction of volatile compounds in “Terrincho”ewe cheese comparison of different fibers[J]. Journal of Chromatography A,2003,1011(1-2):1-9.
[19]衣宇佳,田怀香,郑小平,等.同时蒸馏萃取和固相微萃取法提取国产干酪中风味物质[J].食品与机械,2008,24(2):65-69.
[20]李丽梅,郑振山,何近刚,等.不同品种梨酒挥发性成分的SPME-GC-MS结果比较[J].食品工业科技,2016,11:314-331.
[21]马艳丽,曹雁平,杨贞耐,等. SPME-GC-MS检测不同中西方奶酪的挥发性风味物质及比较[J].食品科学,2013,34(20):103-107.
[22] LI Xiujuan,YE Changwen,HUO Xuelian. Solid-phasemicroextraction using adiglycidyloxycalix
[4]arene coated fiber combined with gas chromatography:Very simple,rapid and sensitive method for the determination of chlorobenzenes in water[J]. MicrochimActa,2010,168:161-167.
[23] STASHENKO E E,MARTíNEZ J R. Sampling volatile compounds from natural products with headspace/solidphase micro-extraction[J]. Journal of Biochemical&Biophysical Methods,2007,70(2):235-242.
[24]孙宝国.食用调香术[M].北京:化学工业出版社,2003:475-494.
[25]栾金水.黄酒中风味物质的研究[J].中国酿造,2002,6:21-24.
[26]邹建凯.气相色谱/质谱研究中国干红葡萄酒香味成分[J].分析化学,2001(4):493-493.
[27] RIU-AUMATELL M,MIRP,SERRA-CAYUELA A,et al. Assessment of the aroma profiles of low-alcohol beers using HS-SPME–GC-MS[J]. Food Research International,2014,57(1):196-202.
[28]张防宇.反相高效液相色谱法测定白酒中乙酸乙酯和苯乙醇的含量[J].酿酒科技,2008,11:108-111.
[29] JUN Hyun-Il,YANG Jae-heon,CHOI Ji-yeon. Changes in volatile flavor compounds in steam-dried Allium hookeriroot[J]. Food Science and Biotechnology,2016,25(5):1 327-1 331.
[30]次顿,达珍,白玛玉珍,等.西藏糌粑主要理化指标及质量现状研究[J].西藏科技,2011(3):18-21.
[31]张琦,薛璐,胡志和.传统酥油研究进展[J].食品工业科技,2013,34(8):361-364.