气相色谱法同时测定啤酒中的甲醛和乙醇
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摘要
本试验首次利用气相色谱法直接同时测定啤酒中甲醛和乙醇的含量,啤酒中的甲醛和乙醇不经过萃取、蒸馏等处理直接用气相色谱法同时进行测定。该方法的线性关系良好,相关系数分别为r_1=0.99924和r_2=0.99911,精密度和重现性较好,精密度值分别为4.19和2.66,加标试验最大回收率值为91.0%,以3倍噪音计算得到方法的检出限分别为0.0065μg/mL和0.0023μg/mL。实验结果表明,采用气相色谱法直接测定啤酒中的甲醛和乙醇操作简单、省时、经济、环保,且省去了传统方法的蒸馏与手工测定比重等繁琐操作,数据可靠,干扰小,检测的灵敏度高,分析速度快,稳定性好,适用于日常啤酒中甲醛和乙醇的检测。
In this study, the content of formaldehyde and ethanol in beer was measured directly(without extraction, distillation and other processing) and simultaneously by gas chromatography for the first time. The linearity of the method was good with the correlation coefficients r_1=0.99924 and r_2=.99911. The precision and reproducibility were satisfactory, and the precision values were 4.19 and 2.66 respectively. The maximum recovery was 91.0 %. The detection limits of triple noise were 0.0065 μg/mL and 0.0023 μg/mL respectively. The experimental results showed that, direct determination of formaldehyde and ethanol content in beer by gas chromatography was simple, time-saving, economical and environment-friendly, and it could eliminate the tedious operation such as distillation and manual measurement. Besides, it had the advantages including reliable data, less interference, high detection sensitivity, fast analysis, and good stability, and it was suitable for routine determination of formaldehyde and ethanol in beer.
In this study, the content of formaldehyde and ethanol in beer was measured directly(without extraction, distillation and other processing) and simultaneously by gas chromatography for the first time. The linearity of the method was good with the correlation coefficients r_1=0.99924 and r_2=.99911. The precision and reproducibility were satisfactory, and the precision values were 4.19 and 2.66 respectively. The maximum recovery was 91.0 %. The detection limits of triple noise were 0.0065 μg/mL and 0.0023 μg/mL respectively. The experimental results showed that, direct determination of formaldehyde and ethanol content in beer by gas chromatography was simple, time-saving, economical and environment-friendly, and it could eliminate the tedious operation such as distillation and manual measurement. Besides, it had the advantages including reliable data, less interference, high detection sensitivity, fast analysis, and good stability, and it was suitable for routine determination of formaldehyde and ethanol in beer.
引文
[1]崔娜,张曼玲,田艳玲.乙酰丙酮法测定啤酒中甲醛含量的研究[J].食品安全质量检测学报,2016(7):906.
[2]陆道礼,林松,陈斌.近红外光谱法快速测定啤酒中乙醇的含量[J].酿酒科技,2005(5):87.
[3]曹桂荣,罗统全,罗广福.某啤酒企业啤酒生产项目职业病危害预评价[J].中国卫生工程学,2014(4):273.
[4]孟悦.啤酒中甲醛浓度定量测定的方法探讨[J].医学信息,2011(5):102.
[5]刘敏,葛红娟,王丹,等.吉林市市售啤酒中甲醛含量的测定与分析[J].酿酒科技,2016(10):103.
[6]张允红.浅谈气相色谱法测定啤酒中痕量甲醛[J].世界最新医学信息文摘,2016(67):285.
[7]BASHEER C,ALNEDHARY A A,RAO B S M,et al.Development and application of porous membraneprotected carbon nanotube micro-solid-phase extraction combined with gas chromatography/mass spectrometry[J].Analytical Chemistry,2006,78(8):2853-2858.
[8]王晓辉,李新,胡志鲜,等.微生物电极法测定啤酒中乙醇含量[J].分析试验室,1998(5):81.
[9]张爱梅,田林芹.动力学分光光度法及荧光光度法测定痕量甲醛[J].分析科学学报,2004(5):519.
[10]EVRAIRIDIS N P,KARAYANNIS M I.Determination of formaldehyde using a kinetic-spctrophotometric method.Part I.Oxidation of p-phenylenediamine with hydrogen peroxide[J].Analyst,1987(6):831.
[11]张娟,钟俊辉,王志沛,等.利用非线性化学指纹图谱法测定啤酒中乙醇含量[J].分析化学,2014(4):559.
[12]宋兴良,震兆岭,朱化雨.动力学光度法测定啤酒中痕量甲醛[J].酿酒科技,2005(7):79.
[13]叶青,魏培莲,尤玉如,等.HPLC法直接测定啤酒中微量甲醛方法的研究[J].食品发酵工业,2006(9):126.
[14]顾秀英,鲍忠定,许荣年,等.衍生气相色谱法测定啤酒中的甲醛[J].检测分析,2008(6):116.
[15]DAHLGRAN J R,JAMESON M N.Determination of formaldehyde and other aldehydes in industrial surfactants by liquid chromatographic separation of their respective 2,4-dinitrophenylhydrazone derivatives[J].Journal-Association of Official Analytical Chemists,1988,71(3):560-563.
[16]陈玉静,徐慧.催化动力学光度法间接测定啤酒中乙醇[J].理化检验(化学分册),2013(49):111.
[17]鲁敏,吕淑清.测定啤酒中甲醛时影响测定结果的因素探讨[J].酿酒科技,2007(7):60.
[18]李军,朱风妹,彭涛.啤酒中甲醛的液相荧光色谱检测方法研究[J].中国食品学报,2007(5):128.
[19]林建.气相色谱法测定甲醛中甲醇含量的研究[J].科学与财富,2015(31):230.
[20]李红,陈苏娟,郭瑞涵,等.绿色食品啤酒标准中甲醛测定方法的探讨[J].酿酒科技,2005(11):81.
[21]黄晓兰,黄芳,林晓珊,等.气相色谱质谱法测定食品中的甲醛[J].分析化学,2004(12):617.
[22]郭荣.气相色谱在食品分析中的应用[J].食品安全导刊,2015(30):49.
[23]顾秀英,鲍忠定,许荣年,等.气相色谱法测定甲醛中的甲醇含量[J].食品研究与开发,2008(6):116.
[2]陆道礼,林松,陈斌.近红外光谱法快速测定啤酒中乙醇的含量[J].酿酒科技,2005(5):87.
[3]曹桂荣,罗统全,罗广福.某啤酒企业啤酒生产项目职业病危害预评价[J].中国卫生工程学,2014(4):273.
[4]孟悦.啤酒中甲醛浓度定量测定的方法探讨[J].医学信息,2011(5):102.
[5]刘敏,葛红娟,王丹,等.吉林市市售啤酒中甲醛含量的测定与分析[J].酿酒科技,2016(10):103.
[6]张允红.浅谈气相色谱法测定啤酒中痕量甲醛[J].世界最新医学信息文摘,2016(67):285.
[7]BASHEER C,ALNEDHARY A A,RAO B S M,et al.Development and application of porous membraneprotected carbon nanotube micro-solid-phase extraction combined with gas chromatography/mass spectrometry[J].Analytical Chemistry,2006,78(8):2853-2858.
[8]王晓辉,李新,胡志鲜,等.微生物电极法测定啤酒中乙醇含量[J].分析试验室,1998(5):81.
[9]张爱梅,田林芹.动力学分光光度法及荧光光度法测定痕量甲醛[J].分析科学学报,2004(5):519.
[10]EVRAIRIDIS N P,KARAYANNIS M I.Determination of formaldehyde using a kinetic-spctrophotometric method.Part I.Oxidation of p-phenylenediamine with hydrogen peroxide[J].Analyst,1987(6):831.
[11]张娟,钟俊辉,王志沛,等.利用非线性化学指纹图谱法测定啤酒中乙醇含量[J].分析化学,2014(4):559.
[12]宋兴良,震兆岭,朱化雨.动力学光度法测定啤酒中痕量甲醛[J].酿酒科技,2005(7):79.
[13]叶青,魏培莲,尤玉如,等.HPLC法直接测定啤酒中微量甲醛方法的研究[J].食品发酵工业,2006(9):126.
[14]顾秀英,鲍忠定,许荣年,等.衍生气相色谱法测定啤酒中的甲醛[J].检测分析,2008(6):116.
[15]DAHLGRAN J R,JAMESON M N.Determination of formaldehyde and other aldehydes in industrial surfactants by liquid chromatographic separation of their respective 2,4-dinitrophenylhydrazone derivatives[J].Journal-Association of Official Analytical Chemists,1988,71(3):560-563.
[16]陈玉静,徐慧.催化动力学光度法间接测定啤酒中乙醇[J].理化检验(化学分册),2013(49):111.
[17]鲁敏,吕淑清.测定啤酒中甲醛时影响测定结果的因素探讨[J].酿酒科技,2007(7):60.
[18]李军,朱风妹,彭涛.啤酒中甲醛的液相荧光色谱检测方法研究[J].中国食品学报,2007(5):128.
[19]林建.气相色谱法测定甲醛中甲醇含量的研究[J].科学与财富,2015(31):230.
[20]李红,陈苏娟,郭瑞涵,等.绿色食品啤酒标准中甲醛测定方法的探讨[J].酿酒科技,2005(11):81.
[21]黄晓兰,黄芳,林晓珊,等.气相色谱质谱法测定食品中的甲醛[J].分析化学,2004(12):617.
[22]郭荣.气相色谱在食品分析中的应用[J].食品安全导刊,2015(30):49.
[23]顾秀英,鲍忠定,许荣年,等.气相色谱法测定甲醛中的甲醇含量[J].食品研究与开发,2008(6):116.