超高效液相色谱法(UPLC)测定猪肉中9种生物胺含量
|
摘要
目的:建立了超高效液相色谱法(UPLC)测定猪肉中色胺、β-苯乙胺、腐胺、尸胺、组胺、章鱼胺、酪胺、亚精胺、精胺含量的方法,并对该检测方法进行优化。方法:样品用5%TCA提取,经丹磺酰氯衍生后,采用C_(18)(2.1 mm×100 mm,1.7μm)色谱柱;以乙腈-10 mmol/L乙酸铵为流动相;流速:0.3 m L/min;检测波长为245 nm,柱温:35℃;进样量3.0μL。结果:在该色谱条件下,9种生物胺在5.0～100.0μg/m L范围内呈良好的线性关系,r≥0.999,最低检测限为0.028～0.29 mg/kg;仪器精密度较好,RSD(n=6)≤3.72%,其平均回收率为70.70%～111.80%。结论:所建立的方法灵敏、准确、简便、重现性好,出峰时间短,对于批量快速准确检测猪肉中生物胺具有很好的应用前景。
Objective: To develop and optimized ultra high pressure liquid chromatography( UPLC) methods for the quantitative determination of tryptamine,β-phenylethylamine,putrescine,cadaverive,histamine,octopamine,tyramine,spermidine and spermine in pork. Methods: The samples were extracted with 5% TCA and derived with dansyl chloride.( 2.1 × 100 mm,1.7 μm) C_(18) column was used.The mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate solution at the flow rate of 0.3 m L/min. The detection wavelength was at 245 nm and the column temperature was 35 ℃.The injection volume was3.0 μL. Results: The linear range of 9 biogenic amines was from 5.0 to 100.0 μg/m L( r≥0.999).The limits of detection were in the range of 0.028～0.29 mg/kg.The relative standard deviation( RSD) of precision was lower than 3.72%.The average recovery was 70.70% ～ 111.80%. Conclusions: The method was simple,accurate,sensitive,reproducible and short peak time. It would have a nice application foreground in a quick,accurate and batch quantity analysis methods of biogenic amines in pork.
Objective: To develop and optimized ultra high pressure liquid chromatography( UPLC) methods for the quantitative determination of tryptamine,β-phenylethylamine,putrescine,cadaverive,histamine,octopamine,tyramine,spermidine and spermine in pork. Methods: The samples were extracted with 5% TCA and derived with dansyl chloride.( 2.1 × 100 mm,1.7 μm) C_(18) column was used.The mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate solution at the flow rate of 0.3 m L/min. The detection wavelength was at 245 nm and the column temperature was 35 ℃.The injection volume was3.0 μL. Results: The linear range of 9 biogenic amines was from 5.0 to 100.0 μg/m L( r≥0.999).The limits of detection were in the range of 0.028～0.29 mg/kg.The relative standard deviation( RSD) of precision was lower than 3.72%.The average recovery was 70.70% ～ 111.80%. Conclusions: The method was simple,accurate,sensitive,reproducible and short peak time. It would have a nice application foreground in a quick,accurate and batch quantity analysis methods of biogenic amines in pork.
引文
[1]Silla Santos MH.Biogenic amines:Their importance in foods[J].Int J Food Microbiol,1996,29(2-3):213-231.
[2]Tassoni A,Germana M,Bagni N. Free and conjugated polyamine content in Citrus sinensis Osbeck,cultivar Brasiliano N.L.92,a Navel orange,at different maturation stages[J]. Food Chemistry,2004,87(4):537-541.
[3] Onal A. A review:Current analytical methods for the determination of biogenic amines in foods[J]. Food Chemistry,2007,103(4):1475-1483.
[4]易丽娟,赵晓娟,白卫东.食品中生物胺检测方法的研究进展[J].食品研究与开发,2016,7(37):197-201.
[5]张春江,杨君娜,王芳芳,等.肉制品中生物胺产生与控制研究进展[J].中国食物与营养,2010(7):17-20.
[6]曾立威,蔡翔宇,吴玉杰,等.超高效液相色谱法同时快速测定多种动物源食品中9种生物胺的含量[J].食品安全质量检测学报,2017,3(8):968-974.
[7]GB 2733-2015食品安全国家标准鲜、冻动物性水产品[S].北京:中国标准出版社,2015.
[8]NY 5073-2006无公害食品水产品中有毒有害物质限量[S].北京:中国标准出版社,2006.
[9]杨静.葡萄酒中生物胺分析方法研究进展[J].食品科学,现代农业科技,2018(7):262-263.
[10]赵玲玲,杜冰,曹炜,等.超高效液相色谱-串联质谱法同时测定蜂蜜中8种生物胺[J].食品工业科技,2018,39(4):228-234.
[11]温永柱,范文来,徐岩.GC-MS法定性白酒中的多种生物胺[J].酿酒,2013,140(1):38-41.
[12]陈玉峰,吴燕燕,李来好,等.腌干鱼制品中8种生物胺测定方法的优化[J].中国渔业质量与标准,2014,4(4):41-48.
[13]杨姗姗.食品中生物胺液相色谱检测方法的建立及应用[D].天津:天津科技大学,2016:3.
[14]GB 5009.208-2016食品安全国家标准食品中生物胺的测定[S].北京:中国标准出版社,2016.
[15]田鑫,刘红,李传勇,等.反相高效液相色谱法同时检测海产品中8种生物胺[J].食品安全质量检测学报,2017,4(8):1171-1177.
[16]罗林,徐振林,沈玉栋,等.食品中生物胺及其检测方法研究进展[J].广东农业学,2013,40(22):119-124.
[17]张宁,王雅琪,王鑫娜,等.前衍生化RP-HPLC法鉴别及测定9种补气药中的生物胺[J].药物分析杂志,2017,37(10):1791-1798.
[18]Patsias A,Chouliara I,Paleologos E K,et al.Relation of biogenic amines to microbial and sensory changes of precooked chicken meat stored aerobically and under modified atmosphere packaging at 4℃[J].European Food Research and Technology,2006,223:683-689.
[19]金邦荃,齐酶,陆裕华,等.苯乙胺与饲料蛋白质水平对猪肉品质和脂肪代谢影响的研究[J].中国饲料,1994(5):13-15.
[20]王真真,李苗云,赵改名,等.真空包装冷却猪肉生物胺与腐败指标的相关性[J].食品科学,2013,37(14):335-339.
[2]Tassoni A,Germana M,Bagni N. Free and conjugated polyamine content in Citrus sinensis Osbeck,cultivar Brasiliano N.L.92,a Navel orange,at different maturation stages[J]. Food Chemistry,2004,87(4):537-541.
[3] Onal A. A review:Current analytical methods for the determination of biogenic amines in foods[J]. Food Chemistry,2007,103(4):1475-1483.
[4]易丽娟,赵晓娟,白卫东.食品中生物胺检测方法的研究进展[J].食品研究与开发,2016,7(37):197-201.
[5]张春江,杨君娜,王芳芳,等.肉制品中生物胺产生与控制研究进展[J].中国食物与营养,2010(7):17-20.
[6]曾立威,蔡翔宇,吴玉杰,等.超高效液相色谱法同时快速测定多种动物源食品中9种生物胺的含量[J].食品安全质量检测学报,2017,3(8):968-974.
[7]GB 2733-2015食品安全国家标准鲜、冻动物性水产品[S].北京:中国标准出版社,2015.
[8]NY 5073-2006无公害食品水产品中有毒有害物质限量[S].北京:中国标准出版社,2006.
[9]杨静.葡萄酒中生物胺分析方法研究进展[J].食品科学,现代农业科技,2018(7):262-263.
[10]赵玲玲,杜冰,曹炜,等.超高效液相色谱-串联质谱法同时测定蜂蜜中8种生物胺[J].食品工业科技,2018,39(4):228-234.
[11]温永柱,范文来,徐岩.GC-MS法定性白酒中的多种生物胺[J].酿酒,2013,140(1):38-41.
[12]陈玉峰,吴燕燕,李来好,等.腌干鱼制品中8种生物胺测定方法的优化[J].中国渔业质量与标准,2014,4(4):41-48.
[13]杨姗姗.食品中生物胺液相色谱检测方法的建立及应用[D].天津:天津科技大学,2016:3.
[14]GB 5009.208-2016食品安全国家标准食品中生物胺的测定[S].北京:中国标准出版社,2016.
[15]田鑫,刘红,李传勇,等.反相高效液相色谱法同时检测海产品中8种生物胺[J].食品安全质量检测学报,2017,4(8):1171-1177.
[16]罗林,徐振林,沈玉栋,等.食品中生物胺及其检测方法研究进展[J].广东农业学,2013,40(22):119-124.
[17]张宁,王雅琪,王鑫娜,等.前衍生化RP-HPLC法鉴别及测定9种补气药中的生物胺[J].药物分析杂志,2017,37(10):1791-1798.
[18]Patsias A,Chouliara I,Paleologos E K,et al.Relation of biogenic amines to microbial and sensory changes of precooked chicken meat stored aerobically and under modified atmosphere packaging at 4℃[J].European Food Research and Technology,2006,223:683-689.
[19]金邦荃,齐酶,陆裕华,等.苯乙胺与饲料蛋白质水平对猪肉品质和脂肪代谢影响的研究[J].中国饲料,1994(5):13-15.
[20]王真真,李苗云,赵改名,等.真空包装冷却猪肉生物胺与腐败指标的相关性[J].食品科学,2013,37(14):335-339.