高效液相色谱法分析发酵肉制品中生物胺
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摘要
建立了高效液相色谱法(high performance liquid chromatography,HPLC)检测发酵肉制品中常见8种生物胺(色胺、β-苯乙胺、腐胺、尸胺、盐酸吡哆胺、组胺、酪胺和精精胺)的柱前衍生-HPLC分析方法,并对其在实际检测中的适用性进行验证。采用5%三氯乙酸作为提取溶剂,提取发酵肉制品中的生物胺,以丹磺酰氯作为衍生试剂,采用Waters Symmetry C_(18)色谱柱(250 mm×4. 6 mm,5μm),乙腈和水(含0. 1%甲酸的0. 01 mol/L乙酸铵溶液)作为流动相进行梯度进样洗脱,流速为0. 8 mL/min,紫外检测器波长为254 nm。结果表明,发酵肉制品中的8种生物胺在37 min内能够进行分离,在0. 05～50μg/mL,8种生物胺均呈现良好的线性相关性(R2>0. 998)。各生物胺3个水平(1. 0、5. 0、10μg/g)加标回收率为83. 34%～111. 4%,相对标准偏差(RSD)均小于4. 85%,8种生物胺检出限为0. 03～0. 21μg/g,定量限为0. 10～0. 69μg/g。
A precolumn derivatization-HPLC method for determining eight biogenic amines( tryptamine,β-phenylethylamine,putrescine,cadaverine,pyridoxamine hydrochloride,histamine,tyramine,and spermine) in fermented meats was established. The applicability of this method in practical was verified and discussed. Biogenic amines in fermented meats were extracted with 5% trichloroacetic acid,and tanshinoyl chloride was used as a derivative reagent. The column used was Waters Symmetry C_(18)( 250 mm × 4. 6 mm,5 μm),acetonitrile and 0. 01 mol/L ammonium acetate solution that contained 0. 1% acetic acid were used as the mobile phase for gradient injection elution. The flow rate was 0. 8 mL/min,and the wavelength of the ultraviolet detector was 254 nm. The results showed that the eight biogenic amines in fermented meats could be separated within 37 min. In the range of 0. 05-50 ug/mL,the eight biogenic amines showed good linear correlations( R2> 0. 998). The recoveries of biogenic amines were83. 34%-111. 4% at three concentrations( 1. 0,5. 0,and 10 μg/g),and the relative standard deviations( RSD)were less than 4. 85%. The detection limits of these eight biogenic amines were 0. 03-0. 21 μg/g,and their quantitative limits were 0. 10-0. 69 μg/g.
A precolumn derivatization-HPLC method for determining eight biogenic amines( tryptamine,β-phenylethylamine,putrescine,cadaverine,pyridoxamine hydrochloride,histamine,tyramine,and spermine) in fermented meats was established. The applicability of this method in practical was verified and discussed. Biogenic amines in fermented meats were extracted with 5% trichloroacetic acid,and tanshinoyl chloride was used as a derivative reagent. The column used was Waters Symmetry C_(18)( 250 mm × 4. 6 mm,5 μm),acetonitrile and 0. 01 mol/L ammonium acetate solution that contained 0. 1% acetic acid were used as the mobile phase for gradient injection elution. The flow rate was 0. 8 mL/min,and the wavelength of the ultraviolet detector was 254 nm. The results showed that the eight biogenic amines in fermented meats could be separated within 37 min. In the range of 0. 05-50 ug/mL,the eight biogenic amines showed good linear correlations( R2> 0. 998). The recoveries of biogenic amines were83. 34%-111. 4% at three concentrations( 1. 0,5. 0,and 10 μg/g),and the relative standard deviations( RSD)were less than 4. 85%. The detection limits of these eight biogenic amines were 0. 03-0. 21 μg/g,and their quantitative limits were 0. 10-0. 69 μg/g.
引文
[1]中商产业研究院.中国肉制品行业前景研究报告[R].中国:中商产业研究院,2018.
[2] LEROY F,VERLUYTEN J,VUYST L D. Functional meat starter cultures for improved sausage fermentation[J]. International Journal of Food Microbiology,2006,106(3):270-285.
[3] International Agency for Research on Cancer(IARC).Consumption of red meat and processed meat:IARC Working Group[R]. Lyon:IARC Monogr Eval Carcinog Risks Hum,2015.
[4] SHALABY A R. Significance of biogenic amines to food safety and human health[J]. Food Research International,1996,29(7):675-690.
[5] BUSTO O,MIRACLE M,GUASCH J,et al. Determination of biogenic amines in wines by high-performance liquid chromatography with on-column fluorescence derivatization[J]. Journal of Chrornatography A,1997,757(1-2):311-318.
[6] TABOR C W,TABOR H. Polyamines[J]. Annual Review of Biochemistry,1984,53:749-790.
[7]冉春霞,陈光静.我国传统发酵肉制品中生物胺的研究进展[J].食品与发酵工业,2017,43(3):285-294.
[8] HERMANDEZ-ORTE P,LAPENA A C,PENA-GALLEGOA A,et al. Biogenic amine determination in wine fermented in oak barrels:factors affecting formation[J].Food Research Intertional,2008,41(7):697-706.
[9] PARENTE E,MATUSCELLI M,GARDINI F,et al. Evolution of microbial populations and biogenic amine production in dry sausages produced in Southern Italy[J]. Journal of Applied Microbiology,2001,90:882-891.
[10] NOUT,M J R. Fermented foods and food safety[J].Food Research International,1994,27:291-298.
[11] HERNáNDEZ-JOVER T,IZQUIERDO-PULIDO M,VECIANA-NOGUéS M T,et al. Biogenic amine and polyamine contents in meat and meat products[J]. Journal of Agricultural and Food Chemistry,1997,45(6):2 098-2 102.
[12] GIOVANNA S,FAUSTO G. Biogenic amines in dry fermented sausages:A review[J]. International Journal of Food Microbiology,2003,88(1):41-54.
[13]张慧,蔡成岗,朱耿杰,等.高效液相色谱法同时测定香肠中6种生物胺[J].中国食品学报,2009,9(4):205-210.
[14]王颖,邱璠,韩北忠,等.食品中的生物胺及其检测方法[J].中国酿造,2011,10:1-5.
[15]廖国周,王桂瑛,曹锦轩,等.宣武火腿中生物胺的HPLC测定[J].食品与发酵工业,2011,37(12):130-132.
[16] ZARGHAMPOUR F,YAMINI Y,BAHARFAR M,et al.Electromembrane extraction of biogenic amines in food samples by a microfluidic-chip system followed by dabsyl derivatization prior to high performance liquid chromatography analysis[J]. Journal of Chromatography A,2018,1 556:21-28.
[17] LIU S J,XU J J,MA C L,et al. A comparative analysis of derivatization strategies for the determination of biogenic amines in sausage and cheese by HPLC[J]. Food Chemistry,2018,266:275-283.
[18] PAPAGEORGIOU M,LAMBROPOULOU D, MORRISON C,et al. Direct solid phase microextraction combined with gas chromatography-mass spectrometry for the determination of biogenic amines in wine[J]. Talanta,2018,183:276-282.
[19] BORBA B M D,ROHRER J S. Determination of biogenic amines in alcoholic beverages by ion chromatography with suppressed conductivity detection and integrated pulsed amperometric detection[J]. Journal of Chromatography A,2007,1 155(1),22-30.
[20] AN D,CHEN Z Q,ZHENG J C,et al. Determination of biogenic amines in oysters by capillary electrophoresis coupled with electrochemiluminescence[J]. Food chemistry,2015,168:1-6.
[21] KIRSCHBAUM J,REBSCHER K,BRüCKNER H. Liquid chromatographic determination of biogenic amines in fermented foods after derivatization with 3, 5-dinitrobenzoyl chloride[J]. Journal of Chromatography A,2000,881(1-2):517-530.
[22] VINCI G,ANTONELLI M L. Biogenic amines:quality index of freshness in red and white meat[J]. Food Control,2002,13(8):519-524.
[23] TRIKI M,JIMéNEZ-COLMENERO F,HERRERO A M,et al. Optimisation of a chromatographic procedure for determining biogenic amine concentrations in meat and meat products employing a cation-exchange column with a postcolumn system[J]. Food Chemistry,2012,130(4):1 066-1 073.
[2] LEROY F,VERLUYTEN J,VUYST L D. Functional meat starter cultures for improved sausage fermentation[J]. International Journal of Food Microbiology,2006,106(3):270-285.
[3] International Agency for Research on Cancer(IARC).Consumption of red meat and processed meat:IARC Working Group[R]. Lyon:IARC Monogr Eval Carcinog Risks Hum,2015.
[4] SHALABY A R. Significance of biogenic amines to food safety and human health[J]. Food Research International,1996,29(7):675-690.
[5] BUSTO O,MIRACLE M,GUASCH J,et al. Determination of biogenic amines in wines by high-performance liquid chromatography with on-column fluorescence derivatization[J]. Journal of Chrornatography A,1997,757(1-2):311-318.
[6] TABOR C W,TABOR H. Polyamines[J]. Annual Review of Biochemistry,1984,53:749-790.
[7]冉春霞,陈光静.我国传统发酵肉制品中生物胺的研究进展[J].食品与发酵工业,2017,43(3):285-294.
[8] HERMANDEZ-ORTE P,LAPENA A C,PENA-GALLEGOA A,et al. Biogenic amine determination in wine fermented in oak barrels:factors affecting formation[J].Food Research Intertional,2008,41(7):697-706.
[9] PARENTE E,MATUSCELLI M,GARDINI F,et al. Evolution of microbial populations and biogenic amine production in dry sausages produced in Southern Italy[J]. Journal of Applied Microbiology,2001,90:882-891.
[10] NOUT,M J R. Fermented foods and food safety[J].Food Research International,1994,27:291-298.
[11] HERNáNDEZ-JOVER T,IZQUIERDO-PULIDO M,VECIANA-NOGUéS M T,et al. Biogenic amine and polyamine contents in meat and meat products[J]. Journal of Agricultural and Food Chemistry,1997,45(6):2 098-2 102.
[12] GIOVANNA S,FAUSTO G. Biogenic amines in dry fermented sausages:A review[J]. International Journal of Food Microbiology,2003,88(1):41-54.
[13]张慧,蔡成岗,朱耿杰,等.高效液相色谱法同时测定香肠中6种生物胺[J].中国食品学报,2009,9(4):205-210.
[14]王颖,邱璠,韩北忠,等.食品中的生物胺及其检测方法[J].中国酿造,2011,10:1-5.
[15]廖国周,王桂瑛,曹锦轩,等.宣武火腿中生物胺的HPLC测定[J].食品与发酵工业,2011,37(12):130-132.
[16] ZARGHAMPOUR F,YAMINI Y,BAHARFAR M,et al.Electromembrane extraction of biogenic amines in food samples by a microfluidic-chip system followed by dabsyl derivatization prior to high performance liquid chromatography analysis[J]. Journal of Chromatography A,2018,1 556:21-28.
[17] LIU S J,XU J J,MA C L,et al. A comparative analysis of derivatization strategies for the determination of biogenic amines in sausage and cheese by HPLC[J]. Food Chemistry,2018,266:275-283.
[18] PAPAGEORGIOU M,LAMBROPOULOU D, MORRISON C,et al. Direct solid phase microextraction combined with gas chromatography-mass spectrometry for the determination of biogenic amines in wine[J]. Talanta,2018,183:276-282.
[19] BORBA B M D,ROHRER J S. Determination of biogenic amines in alcoholic beverages by ion chromatography with suppressed conductivity detection and integrated pulsed amperometric detection[J]. Journal of Chromatography A,2007,1 155(1),22-30.
[20] AN D,CHEN Z Q,ZHENG J C,et al. Determination of biogenic amines in oysters by capillary electrophoresis coupled with electrochemiluminescence[J]. Food chemistry,2015,168:1-6.
[21] KIRSCHBAUM J,REBSCHER K,BRüCKNER H. Liquid chromatographic determination of biogenic amines in fermented foods after derivatization with 3, 5-dinitrobenzoyl chloride[J]. Journal of Chromatography A,2000,881(1-2):517-530.
[22] VINCI G,ANTONELLI M L. Biogenic amines:quality index of freshness in red and white meat[J]. Food Control,2002,13(8):519-524.
[23] TRIKI M,JIMéNEZ-COLMENERO F,HERRERO A M,et al. Optimisation of a chromatographic procedure for determining biogenic amine concentrations in meat and meat products employing a cation-exchange column with a postcolumn system[J]. Food Chemistry,2012,130(4):1 066-1 073.
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