柱前衍生-高效液相色谱-二极管阵列法测定葡萄酒中组胺含量
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摘要
目的建立柱前衍生-高效液相色谱-二极管阵列法(high performance liquid chromatography-diode arraydetector,HPLC-DAD)测定葡萄酒中组胺含量的方法。方法将葡萄酒样品与10mg/mL的丹磺酰氯在70℃柱前衍生10min,衍生样品以乙腈和0.01mol/L乙酸铵溶液(含0.1%乙酸)为流动相进行等度洗脱,于波长254 nm处进行检测。结果该方法的标准曲线回归方程为Y=0.0319X+0.00059, 0.1～100μg/mL的线性范围内,组胺标准品峰面积与内标物峰面积的比值与组胺含量线性关系良好,相关系数r2为0.9987,回收率为92.3%～105.2%,检出限为0.05μg/mL。结论该方法操作简便、准确度高,适用于葡萄酒中组胺含量测定。
Objective To establish a method for determination of histamine in wine by pre-column derivatization-high performance liquid chromatography-diode array detector(HPLC-DAD).Methods The wine sample was derigaved with 10 mg/mL dansyl chloride for 10 min at 70 ℃.The derived sample was detected at 254 nm after isocratic elution with acetonitrile and 0.01 mol/L ammonium acetate solution(containing 0.1% acetic acid) as the mobile phase.Results The standard curve regression equation of this method was Y=0.0319 X+0.00059,with the linear range of 0.1-100 μg/mL.The ratio of the peak area of the histamine standard to the peak area of the internal standard was linearly related to the histamine content,the correlation coefficient r2 was 0.9987,the recovery was 92.3%-105.2%,and the limit of detection was 0.05 μg/mL.Conclusion This method is simple,rapid and accurate,which is suitable for the determination of histamine in wine.
Objective To establish a method for determination of histamine in wine by pre-column derivatization-high performance liquid chromatography-diode array detector(HPLC-DAD).Methods The wine sample was derigaved with 10 mg/mL dansyl chloride for 10 min at 70 ℃.The derived sample was detected at 254 nm after isocratic elution with acetonitrile and 0.01 mol/L ammonium acetate solution(containing 0.1% acetic acid) as the mobile phase.Results The standard curve regression equation of this method was Y=0.0319 X+0.00059,with the linear range of 0.1-100 μg/mL.The ratio of the peak area of the histamine standard to the peak area of the internal standard was linearly related to the histamine content,the correlation coefficient r2 was 0.9987,the recovery was 92.3%-105.2%,and the limit of detection was 0.05 μg/mL.Conclusion This method is simple,rapid and accurate,which is suitable for the determination of histamine in wine.
引文
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[3]冉春霞,陈光静,胡江.HPLC法测定渝东南地区传统土家特色酸鲊肉中的组胺含量[J].食品科学,2017,38(12):286-231.Ran CX,Chen GJ,Hu J.Determination of histamine content in Suanzharou,a unique and traditional fermented meat product of the tujia nationality in southeastern Chongqing by high performance liquid chromatography[J].Food Sci,2017,38(12):286-231.
[4]魏雷,吉姆·哈迪,曾令文.果酒中组胺含量快速检测方法研究[J].食品科技,2018,43(7):327-331.Wei L,Jimu HD,Zeng LW.Rapid detection method of histamine content in fruit wine[J].Food Sci Technol,2018,43(7):327-331.
[5]赵宇明.分光光度法快速测定水产品中组胺的含量[J].食品研究与开发,2014,35(8):94-96.Zhao YM.Rapid detection histamine content in aquatic product using spectrophotometry[J].Food Res Dev,2014,35(8):94-96.
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[9]周婵媛,赵晓娟,杨春婷.化学修饰电极检测食品中组胺的研究进展[J].食品与发酵工业,2018,44(6):281-286.Zhou CY,Zhao XJ,Yang CT.Research progress in chemically modified electrodes for determination of histamine in foods[J].Food Ferm Ind,2018,44(6):281-286.
[10]廖国周,王桂瑛,曹锦轩,等.宣威火腿中生物胺的HPLC测定[J].食品与发酵工业,2011,37(12):130-132.Liao GZ,Wang GY,Cao JX,et al.Detection of biogenic amines in Xuanwei ham by HPLC[J].Food Ferm Ind,2011,37(12):130-132.
[11]郝宏兰.水产品中组胺的测定方法研究[J].食品科学,2000,21(8):46-48.Hao HL.Study on the determination method of histamine in aquatic products[J].Food Sci,2000,21(8):46-48.
[12]沈念原,王秀芹.高效液相色谱法测定葡萄酒中生物胺的含量[J].食品工业科技,2011,32(4):394-396.Shen NY,Wang XQ.Determination of biogenic amines in wine by high performance liquid chromatography[J].Sci Technol Food Ind,2011,32(4):394-396.
[13]王瑞,许超丽,乔丹,等.新疆四大优势产区葡萄酒中生物胺含量的测定[J].中国酿造,2018,37(8):178-181.Wang R,Xu CL,Qiao D,et al.Determination of biogenic amines in wines from four major production areas in Xinjiang[J].China Brew,2018,37(8):178-181.
[14]胡家伟,高榕,曹敏杰,等.水产食品中组胺的丹磺酰氯柱前衍生反相高效液相色谱测定方法的建立及应用[J].食品科学,2014,35(8):283-288.Hu JW,Gao R,Cao MJ,et al.Establishment and application of dansyl chloride precolumn derivatization RP-HPLC for determination of histamine in aquatic products[J].Food Sci,2014,35(8):283-288.
[15]Legua CM,Falco PC,Cabeza AS,et al.Urine polyamines determination using dansyl chloride derivatization in solid-phase extraction cartridges and HPLC[J].Analyst,1999,124(4):477-482.
[16]GB 5009.208-2016食品安全国家标准食品中生物胺的测定[S].GB 5009.208-2016 National food safety standard-Determination of biogenic amines in food[S].
[2]李志军,吴永宁,薛长湖.生物胺与食品安全[J].食品与发酵工业,2004,30(10):87-94.Li ZJ,Wu YN,Xue CH.Biogenic amines and food safety[J].Food Ferm Ind,2004,30(10):87-94.
[3]冉春霞,陈光静,胡江.HPLC法测定渝东南地区传统土家特色酸鲊肉中的组胺含量[J].食品科学,2017,38(12):286-231.Ran CX,Chen GJ,Hu J.Determination of histamine content in Suanzharou,a unique and traditional fermented meat product of the tujia nationality in southeastern Chongqing by high performance liquid chromatography[J].Food Sci,2017,38(12):286-231.
[4]魏雷,吉姆·哈迪,曾令文.果酒中组胺含量快速检测方法研究[J].食品科技,2018,43(7):327-331.Wei L,Jimu HD,Zeng LW.Rapid detection method of histamine content in fruit wine[J].Food Sci Technol,2018,43(7):327-331.
[5]赵宇明.分光光度法快速测定水产品中组胺的含量[J].食品研究与开发,2014,35(8):94-96.Zhao YM.Rapid detection histamine content in aquatic product using spectrophotometry[J].Food Res Dev,2014,35(8):94-96.
[6]曹利瑞,朱松,俞剑燊,等.黄酒中9种生物胺的高效液相色谱分析法[J].食品科学,2016,37(4):103-106.Cao LR,Zhu S,Yu JS,et al.Development of an analytical method for nine biogenic amines in Chinese yellow wine by HPLC[J].Food Sci,2016,37(4):103-106.
[7]Huang J,Gan N,Lv F,et al.Environmentally friendly solid-phase microextraction coupled with gas chromatography and mass spectrometry for the determination of biogenic amines in fish samples[J].J Separ Sci,2016,(39):4384-4390.
[8]郑海松,杨小娇.进出口食品中组胺的ELISA快速测定[J].食品工业,2011,(10):110-112.Zheng HS,Yang XJ.Rapid detection of histamine in import and export food by ELISA method[J].Food Ind,2011,(10):110-112.
[9]周婵媛,赵晓娟,杨春婷.化学修饰电极检测食品中组胺的研究进展[J].食品与发酵工业,2018,44(6):281-286.Zhou CY,Zhao XJ,Yang CT.Research progress in chemically modified electrodes for determination of histamine in foods[J].Food Ferm Ind,2018,44(6):281-286.
[10]廖国周,王桂瑛,曹锦轩,等.宣威火腿中生物胺的HPLC测定[J].食品与发酵工业,2011,37(12):130-132.Liao GZ,Wang GY,Cao JX,et al.Detection of biogenic amines in Xuanwei ham by HPLC[J].Food Ferm Ind,2011,37(12):130-132.
[11]郝宏兰.水产品中组胺的测定方法研究[J].食品科学,2000,21(8):46-48.Hao HL.Study on the determination method of histamine in aquatic products[J].Food Sci,2000,21(8):46-48.
[12]沈念原,王秀芹.高效液相色谱法测定葡萄酒中生物胺的含量[J].食品工业科技,2011,32(4):394-396.Shen NY,Wang XQ.Determination of biogenic amines in wine by high performance liquid chromatography[J].Sci Technol Food Ind,2011,32(4):394-396.
[13]王瑞,许超丽,乔丹,等.新疆四大优势产区葡萄酒中生物胺含量的测定[J].中国酿造,2018,37(8):178-181.Wang R,Xu CL,Qiao D,et al.Determination of biogenic amines in wines from four major production areas in Xinjiang[J].China Brew,2018,37(8):178-181.
[14]胡家伟,高榕,曹敏杰,等.水产食品中组胺的丹磺酰氯柱前衍生反相高效液相色谱测定方法的建立及应用[J].食品科学,2014,35(8):283-288.Hu JW,Gao R,Cao MJ,et al.Establishment and application of dansyl chloride precolumn derivatization RP-HPLC for determination of histamine in aquatic products[J].Food Sci,2014,35(8):283-288.
[15]Legua CM,Falco PC,Cabeza AS,et al.Urine polyamines determination using dansyl chloride derivatization in solid-phase extraction cartridges and HPLC[J].Analyst,1999,124(4):477-482.
[16]GB 5009.208-2016食品安全国家标准食品中生物胺的测定[S].GB 5009.208-2016 National food safety standard-Determination of biogenic amines in food[S].