介质阻挡放电氦等离子体-气相色谱测定绿豆中脂肪酸含量
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摘要
基于介质阻挡放电氦等离子体-气相色谱结合微型样品前处理方式,建立绿豆中脂肪酸含量的快速测定方法,采用石英毛细管柱HP-88(100 m×0.25 mm,0.25μm)(88%-氰丙基/芳基-聚硅氧烷固定液),载气为超纯氦气(纯度99.999 9%),载气流量为1.5 mL/min,柱温为程序升温,进样口温度250℃,隔垫吹扫流量为3 mL/min,分流比为1∶60,检测器温度为280℃,等离子体放电气体流量为40 mL/min,进样体积为1μL;样品中目标物采用异辛烷萃取,氢氧化钾-甲醇甲酯化后上机分析。实验结果表明,绿豆样品中8种脂肪酸甲酯检测灵敏度在0.105～0.196μg/mL之间,相对标准偏差在1.04%～1.35%之间。所建方法所需样品量及化学试剂少,样品前处理简单快速,重现性好,能够精确测定绿豆中脂肪酸含量。
A rapid method for the determination of the fatty acid content in mung bean was established based on gas chromatography(GC) with a dielectric barrier discharge ionization detector combined with micro sample pretreatment.The chromatographic column adopted in this method was HP-88(100 m × 0.25 mm, 0.25 μm)(88% cyanopropyl/aryl polysiloxane stationary liquid), and the carrier gas was super pure helium(purity 99.999 9 %) with a ?ow rate of 1.5 mL/min.The column temperature was programmed. The inlet temperature was 250 ℃, septum purge ?ow rate 3 mL/min, and split ratio 1:60. The detector temperature was 280 ℃ and plasma discharge gas flow rate 40 mL/min. The sample injection volume was 1 μL. The target compounds in samples were extracted with isooctane and esteri?ed with potassium hydroxide/methanol before analysis. The results showed that the sensitivity for 8 fatty acids in mung bean samples ranged from 0.105 to 0.196 μg/m L, with relative standard deviations ranging from 1.04% to 1.35%. The established method required very small amounts of samples and chemical reagents, and the sample pretreatment was simple, rapid and reproducible, and thus this method could accurately measure the content of fatty acids in mung bean.
A rapid method for the determination of the fatty acid content in mung bean was established based on gas chromatography(GC) with a dielectric barrier discharge ionization detector combined with micro sample pretreatment.The chromatographic column adopted in this method was HP-88(100 m × 0.25 mm, 0.25 μm)(88% cyanopropyl/aryl polysiloxane stationary liquid), and the carrier gas was super pure helium(purity 99.999 9 %) with a ?ow rate of 1.5 mL/min.The column temperature was programmed. The inlet temperature was 250 ℃, septum purge ?ow rate 3 mL/min, and split ratio 1:60. The detector temperature was 280 ℃ and plasma discharge gas flow rate 40 mL/min. The sample injection volume was 1 μL. The target compounds in samples were extracted with isooctane and esteri?ed with potassium hydroxide/methanol before analysis. The results showed that the sensitivity for 8 fatty acids in mung bean samples ranged from 0.105 to 0.196 μg/m L, with relative standard deviations ranging from 1.04% to 1.35%. The established method required very small amounts of samples and chemical reagents, and the sample pretreatment was simple, rapid and reproducible, and thus this method could accurately measure the content of fatty acids in mung bean.
引文
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[11]刘俊英,谢国莉,危晴,等.小米中脂肪酸的GC-MS法测定及营养价值分析[J].食品研究与开发,?2012,?33(2):?165-167;?168.?DOI:10.3969/j.issn.1005-6521.2012.02.049.
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[17]洪欢欢,赵鹏,宁录胜,等.基于新型介质阻挡放电离子源的药物快速检测方法研究[J].分析化学,2017,45(10):1529-1534.DOI:10.11895/j.issn.0253-3820.170360.
[18]李福芬,古锐帆,孙赟珑,等.气相色谱法BID检测器上TO-14AVOCs标准气体分析方法的研究[J].低温与特气,2014,32(6):37-42.DOI:10.3969/j.issn.1007-7804.2014.06.009.
[19]刘慧,时自立,李峰.DID气相色谱法分析精丙烯中微量永久性气体杂质[J].河南化工,2015,32:54-57.DOI:10.14173/j.cnki.hnhg.2015.08.015.
[20]方华,周朋云,庄鸿涛.氦离子化检测器(PDHID)与火焰离子化检测器(FID)在高纯气体分析中的性能比较[J].低温与特气,2011,29(1):33-42.DOI:10.3969/j.issn.1007-7804.2011.01.010.
[21]刘晓红,于大秋,任越,等.脉冲放电氦离子化气相色谱仪在特种气体分析中的应用[J].低温与特气,2016,34(1):32-38.DOI:10.3969/j.issn.1007-7804.2016.01.008.
[22]李富勇,郭东方,金伟,等.气相色谱用氦等离子体离子化检测器研究进展[J].分析科学学报,2012,28(2):279-284.
[23]田肖丹,杨文军,刘淼,等.气相色谱用氦直流等离子体离子化检测器的研究[J].化学学报,1996,54(7):691-696.DOI:10.3969/j.issn.1006-3536.2009.05.023.
[24]田甜,武俊瑞,岳喜庆,等.传统豆酱中脂肪酸酯化方法的选择与组成分析[J].食品科学,2014,35(18):78-83.DOI:10.7506/spkx1002-6630-201418015.
[25]张耀广,王玉英,柴艳兵,等.GC-MS法测定生鲜牛乳脂肪酸组成及含量的研究[J].食品研究与开发,2015,36(13):99-102.DOI:10.3969/j.issn.1005-6521.2015.13.028.
[26]黄丽,李金林,王楚芳,等.婴幼儿配方谷粉中多组分反式脂肪酸的同步测定[J].食品与机械,2018,34(2):57-57;137.DOI:10.13652/j.issn.1003-5788.2018.02.012.
[27]杨晓琴,黄元波,郑云武,等.水红木果油的超声辅助提取与脂肪酸组成研究[J].西南林业大学学报,2018,38(1):169-174.DOI:10.11929/j.issn.2095-1914.2018.01.026.
[28]陈展宇,常雨婷,付良帅,等.新老大豆品种不同冠层籽粒脂肪酸含量与叶片光合速率研究[J].西北农林科技大学学报(自然科学版),2018,46(1):95-102.DOI:10.13207/j.cnki.jnwafu.2018.01.013.
[29]钱宗耀,刘河疆,张维维,等.气质联用-内标法测定豆类中脂肪酸含量及因子分析[J].中国粮油学报,?2017,?32(2):?130-134;?139.?DOI:10.3969/j.issn.1003-0174.2017.02.023.
[30]谢庆方,张丽霞,张振山.不同品种红麻籽油的品质及微量成分分析[J].河南工业大学学报(自然科学版),2018,39(1):39-44.DOI:10.16433/j.cnki.issn1673-2383.2018.01.007.
[31]庄海旗,刘江琴,崔燎,等.南海海域8种金线鱼肌肉的脂肪酸分析[J].现代食品科技,2018,34(3):218-225.DOI:10.13982/j.mfst.1673-9078.2018.03.032.
[2]蔡晓宁,张来林,陶琳岩.不同储藏条件下绿豆品质变化规律研究[J].河南工业大学学报(自然科学版),2016,37(2):16-21.DOI:10.16433/j.cnki.issn1673-2383.2016.02.004.
[3]马秀杰.间作对绿豆生物性状、产量和品质的影响[J].核农学报,2014,28(3):546-551.DOI:10.11869/j.issn.100-8551.2014.03.0546.
[4]TIAN Q,ZHANG W L,LI Q,et al.Research progress of quality characteristics and comprehensive utilization of mung beans[J].Agricultural Science&Technology,2017,18(1):127-133;136.DOI:10.16175/j.cnki.1009-4229.2017.01.029.
[5]谢艳华,谢靓,李跑,等.豆类脂肪酸分析方法研究现状及进展[J].食品与机械,2016,32(12):213-217.DOI:10.13652/j.issn.1003-5788.2016.12.046.
[6]杨亚琴,周其芳,刘进玺,等.气相色谱法测定食用豆中主要脂肪酸含量[J].食品安全质量检测学报,2017,8(2):574-578.DOI:10.3969/j.issn.2095-0381.2017.02.035.
[7]范胜栩,李斌,孙君明,等.气相色谱法定量检测大豆5种脂肪酸[J].中国油料作物学报,2015(4):548-553.DOI:10.7505/j.issn.1007-9084.2015.04.017.
[8]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.DOI:10.7506/spkx1002-6630-201614022.
[9]雷雨和,眭玥,骞宇,等.永川毛霉型豆豉中脂肪酸提取力法比较研究[J].中国调味品,2014(5):114-117.DOI:10.3969/j.issn.1000-9973.2014.05.030.
[10]蒋立文,郑兵福,李白玉,等.四棱豆油脂、脂肪酸、蛋白质、氨基酸的分析[J].食品科学,2010,31(10):231-234.
[11]刘俊英,谢国莉,危晴,等.小米中脂肪酸的GC-MS法测定及营养价值分析[J].食品研究与开发,?2012,?33(2):?165-167;?168.?DOI:10.3969/j.issn.1005-6521.2012.02.049.
[12]王新新.介质阻挡放电及其应用[J].高电压技术,2009,35(1):1-11.
[13]KUNZE K,MICIEA M,FRANZKE J,et al.The dielectric barrier discharge as a detector for gas chromatography[J].Spectrochimica Acta(Part B),2003,58:1435-1443.DOI:10.1016/S0584-8547(03)00104-6.
[14]MIRABELLI M F,WOLF J C,ZENOBI R.Atmospheric pressure soft ionization for gas chromatography with dielectric barrier discharge ionization-mass spectrometry(GC-DBDI-MS)[J].Analyst,2017,142:1909-1915.DOI:10.1039/c7an00245a.
[15]FRANCHINA F A,MAIMONE M,SCIARRONE D,et al.Evaluation of a novel helium ionization detector within the context of(low-)flow modulation comprehensive two-dimensional gas chromatography[J].Journal of Chromatography A,2015,1402:102-109.DOI:10.1016/j.chroma.2015.05.013.
[16]ANSGAR T K,TORBEN L,STEFAN Z.A sensitive gas chromatography detector based on atmospheric pressure chemical ionization by a dielectric barrier discharge[J].Journal of Chromatography A,2017,1483:120-126.DOI:10.1016/j.chroma.2016.12.071.
[17]洪欢欢,赵鹏,宁录胜,等.基于新型介质阻挡放电离子源的药物快速检测方法研究[J].分析化学,2017,45(10):1529-1534.DOI:10.11895/j.issn.0253-3820.170360.
[18]李福芬,古锐帆,孙赟珑,等.气相色谱法BID检测器上TO-14AVOCs标准气体分析方法的研究[J].低温与特气,2014,32(6):37-42.DOI:10.3969/j.issn.1007-7804.2014.06.009.
[19]刘慧,时自立,李峰.DID气相色谱法分析精丙烯中微量永久性气体杂质[J].河南化工,2015,32:54-57.DOI:10.14173/j.cnki.hnhg.2015.08.015.
[20]方华,周朋云,庄鸿涛.氦离子化检测器(PDHID)与火焰离子化检测器(FID)在高纯气体分析中的性能比较[J].低温与特气,2011,29(1):33-42.DOI:10.3969/j.issn.1007-7804.2011.01.010.
[21]刘晓红,于大秋,任越,等.脉冲放电氦离子化气相色谱仪在特种气体分析中的应用[J].低温与特气,2016,34(1):32-38.DOI:10.3969/j.issn.1007-7804.2016.01.008.
[22]李富勇,郭东方,金伟,等.气相色谱用氦等离子体离子化检测器研究进展[J].分析科学学报,2012,28(2):279-284.
[23]田肖丹,杨文军,刘淼,等.气相色谱用氦直流等离子体离子化检测器的研究[J].化学学报,1996,54(7):691-696.DOI:10.3969/j.issn.1006-3536.2009.05.023.
[24]田甜,武俊瑞,岳喜庆,等.传统豆酱中脂肪酸酯化方法的选择与组成分析[J].食品科学,2014,35(18):78-83.DOI:10.7506/spkx1002-6630-201418015.
[25]张耀广,王玉英,柴艳兵,等.GC-MS法测定生鲜牛乳脂肪酸组成及含量的研究[J].食品研究与开发,2015,36(13):99-102.DOI:10.3969/j.issn.1005-6521.2015.13.028.
[26]黄丽,李金林,王楚芳,等.婴幼儿配方谷粉中多组分反式脂肪酸的同步测定[J].食品与机械,2018,34(2):57-57;137.DOI:10.13652/j.issn.1003-5788.2018.02.012.
[27]杨晓琴,黄元波,郑云武,等.水红木果油的超声辅助提取与脂肪酸组成研究[J].西南林业大学学报,2018,38(1):169-174.DOI:10.11929/j.issn.2095-1914.2018.01.026.
[28]陈展宇,常雨婷,付良帅,等.新老大豆品种不同冠层籽粒脂肪酸含量与叶片光合速率研究[J].西北农林科技大学学报(自然科学版),2018,46(1):95-102.DOI:10.13207/j.cnki.jnwafu.2018.01.013.
[29]钱宗耀,刘河疆,张维维,等.气质联用-内标法测定豆类中脂肪酸含量及因子分析[J].中国粮油学报,?2017,?32(2):?130-134;?139.?DOI:10.3969/j.issn.1003-0174.2017.02.023.
[30]谢庆方,张丽霞,张振山.不同品种红麻籽油的品质及微量成分分析[J].河南工业大学学报(自然科学版),2018,39(1):39-44.DOI:10.16433/j.cnki.issn1673-2383.2018.01.007.
[31]庄海旗,刘江琴,崔燎,等.南海海域8种金线鱼肌肉的脂肪酸分析[J].现代食品科技,2018,34(3):218-225.DOI:10.13982/j.mfst.1673-9078.2018.03.032.
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