高效液相色谱法测定豆制品中的甲醛
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摘要
目的建立高效液相色谱法测定豆制品中甲醛含量的分析方法。方法样品粉碎后,采用乙腈-2,4-二硝基苯肼和磷酸二氢钠溶液的混合体系为衍生溶液提取样品中的甲醛,生成的产物经色谱柱WelchXB-C_(18)(4.6mm×250mm,5μm)洗脱,流动相为乙腈-水(70:30,V:V),柱温为35℃,流速为0.8mL/min;检测波长为355 nm,高效液相色谱法检测。结果甲醛质量浓度在0～3.0μg/mL范围内呈良好线性,相关系数r~2为0.9999,在2、10和40μg3个加标水平的回收率为87.22%～93.92%,相对标准偏差为0.75%～3.87%,检出限为0.05mg/kg。结论本方法灵敏度高,操作简便,准确可靠,适合于测定豆制品中甲醛的含量。
Objective To establish a method for determination of formaldehyde in soybean product by high performance liquid chromatography(HPLC). Methods The formaldehyde in the smashed sample was extracted from the derivatized solution which was a mixed system of acetonitrile-2,4-dinitrophenylhydrazine and sodium dihydrogen phosphate solution, and then the product was eluted by a column of Welch XB-C_(18)(4.6 mm×250 mm, 5 μm) with the mobile phase of acetonitrile-water(70:30, V:V) at 35 ℃, and the flow rate was 0.8 mL/min. The detection wavelength was 355 nm, and it was detected by high performance liquid chromatography. Results Under optimmal experimental conditions, good linearity was observed in the range of 0-3.0 μg/mL with a correlation coefficient(r~2) of 0.9999. The recoveries of formaldehyde at 3 levels(2, 10 and 40 μg) were 87.22%-93.92% and the relative standard deviations(RSD) were between 0.75% and 3.87%. The limit of detection was 0.05 mg/kg. Conclusion The established method is simple, rapid, reliable and accurate, which is suitable for the detection of formaldehyde in soybean product.
Objective To establish a method for determination of formaldehyde in soybean product by high performance liquid chromatography(HPLC). Methods The formaldehyde in the smashed sample was extracted from the derivatized solution which was a mixed system of acetonitrile-2,4-dinitrophenylhydrazine and sodium dihydrogen phosphate solution, and then the product was eluted by a column of Welch XB-C_(18)(4.6 mm×250 mm, 5 μm) with the mobile phase of acetonitrile-water(70:30, V:V) at 35 ℃, and the flow rate was 0.8 mL/min. The detection wavelength was 355 nm, and it was detected by high performance liquid chromatography. Results Under optimmal experimental conditions, good linearity was observed in the range of 0-3.0 μg/mL with a correlation coefficient(r~2) of 0.9999. The recoveries of formaldehyde at 3 levels(2, 10 and 40 μg) were 87.22%-93.92% and the relative standard deviations(RSD) were between 0.75% and 3.87%. The limit of detection was 0.05 mg/kg. Conclusion The established method is simple, rapid, reliable and accurate, which is suitable for the detection of formaldehyde in soybean product.
引文
[1]黄种乾,李亚楠,高丽霞,等.食品中甲醛分析方法研究进展[J].食品安全质量检测学报,2015,6(12):4712-4717.Huang ZQ,Li YN,Gao LX,et al.Research advances of analysis techniques of formaldehyde in foods[J].J Food Saf Qual,2015,6(12):4712-4717.
[2]李忠军,邹训重,黎彧,等.甲醛测定方法的进展概述[J].广东微量元素科学,2014,21(6):28-32.Li ZJ,Zou XZ,Li Y,et al.The research summary of formaldehyde determination methods[J].Guangdong Trac Elem Sci,2014,21(6):28-32.
[3]靳红果,刘华琳,张瑞,等.食品中甲醛及其检测方法[J].食品工业科技,2013,34(19):373-376.Jin HG,Liu HL,Zhang R,et al.Review of analytical methods for the determination of formaldehyde in food[J].Sci Technol Food Ind,2013,34(19):373-376.
[4]李俊,刘辉,刘嘉,等.乙酰丙酮分光光度法检测果蔬中甲醛含量的改进研究[J].食品科技,2016,41(9):289-294.Li J,Liu H,Liu J,et al.Improvement on acetylacetone spectrophotometry for formaldehyde detection in fruits and vegetables[J].Food Sci Technol,2016,41(9):289-294.
[5]王冬芬,李道敏.乙酰丙酮法测定香菇中的甲醛[J].河南预防医学杂志,2014,25(1):40-42.Wang DF,Li DM.Determination of formaldehyde in mushrooms acetyl acetone method[J].Henan J Prev Med,2014,25(1):40-42.
[6]李俊,吕都,陈中爱,等.果蔬中甲醛提取方法的优选研究[J].食品工业,2017,38(1):32-36.Li J,Lv D,Chen ZA,et al.Optimization research on extract methods of formaldehyde in fruits and vegetables[J].Food Ind,2017,38(1):32-36.
[7]邵仕萍,相大鹏,李华斌,等.乙酰丙酮衍生化高效液相色谱-荧光检测法测定食品中的甲醛[J].食品科学,2015,36(16):241-245.Shao SP,Xiang DP,Li HB,et al.Determination of formaldehyde in foods by high-performance liquid chromatography with fluorescence detection through derivatization with acetylacetone[J].Food Sci,2015,36(16):241-245.
[8]张艳艳,潘小红,张礼红.高效液相色谱法测定食品中甲醛次硫酸氢钠含量[J].食品安全质量检测学报,2017,8(4):1470-1474.Zhang YY,Pan XH,Zhang LH.Determination of sodium formaldehyde sulfoxylate in food by highperformance liquid chromatography[J].J Food Saf Qual,2017,8(4):1470-1474.
[9]甘凝岚,颜春荣,徐春祥.高效液相色谱法测定鸭血制品中甲醛含量[J].食品科学,2014,35(12):204-207.Gan NL,Yan CR,Xu CX.Determination of formaldehyde in duck blood products by HPLC[J].Food Sci,2014,35(12):204-207.
[10]张莉,江丰,范志勇,等.气相色谱-串联质谱联用仪测定大豆及大豆制品中甲醛含量[J].食品研究与开发,2016,37(11):153-156.Zhang L,Jiang F,Fan ZY,et al.Determination of formaldehyde in soybean and soybean product using gas chromatography-tandem mass spectrometry[J].Food Res Dev,2016,37(11):153-156.
[11]唐穂平.柱前衍生高效液相色谱法检测水产品中甲醛的含量[J].食品安全质量检测学报,2016,7(7):2931-2936.Tang SP.Determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization[J].JFood Saf Qual,2016,7(7):2931-2936.
[12]孟繁磊,牛红红,宋志峰,等.高效液相色谱法测定黑木耳中甲醛含量[J].食品工业,2017,38(6):311-313.Meng FL,Niu HH,Song ZF,et al.Determination of formaldehyde content in black fungus by HPLC[J].Food Ind,2017,38(6):311-313.
[13]刘瑞芳,廖和菁,胡礼渊,等.高效液相色谱法测定进口鱼柳中的吊白块方法研究[J].食品研究与开发,2016,37(1):164-166.Liu RF,Liao HJ,Hu LY,et al.Study on the determination method of the sodium formaldehyde fulfoxylate in imported fish fillet by HPLC[J].Food Res Dev,2016,37(1):164-166.
[14]DB41/T 424-2005食品中甲醛合次硫酸氢钠(吊白块)的测定[S].DB41/T 424-2005 Determination of sodium formaldehyde sulfoxylate(hanging white block)in food[S].
[15]NY/T 1283-2007香菇中甲醛含量的测定[S].NY/T 1283-2007 Determination of Formaldehyde Content in Lentinula edodes[S].
[16]GB/T 21126-2007小麦粉与大米粉及其制品中甲醛次硫酸氢钠含量的测定[S].GB/T 21126-2007 Determination of sodium formaldehyde suifoxylate in grain products[S].
[17]SC/T 3025-2006水产品中甲醛的测定[S].SC/T 3025-2006 Determination of formaldehyde in aquatic products[S].
[18]魏昭,吴蕊,梁勃,等.2,4-二硝基苯肼衍生化-高效液相色谱法测定面粉中的甲醛[J].食品安全导刊,2016,(11):67-68.Wei Z,Wu R,Liang B,et al.Determination of formaldehyde in flour by high performance liquid chromatography with 2,4-dinitrophenylhydrazine derivatization[J].China Food Saf Magaz,2016,(11):67-68.
[19]吕春华,陈梅,陈笑梅,等.衍生液提取-高效液相色谱法测定食品中甲醛[J].理化检验-化学分册,2011,47(9):1005-1008.Lv CH,Chen M,Chen XM,et al.HPLC determination of formaldehyde in foodstuffs by extraction with derivation solution[J].Ptca(Part B:Chem Anal),2011,47(9):1005-1008.
[2]李忠军,邹训重,黎彧,等.甲醛测定方法的进展概述[J].广东微量元素科学,2014,21(6):28-32.Li ZJ,Zou XZ,Li Y,et al.The research summary of formaldehyde determination methods[J].Guangdong Trac Elem Sci,2014,21(6):28-32.
[3]靳红果,刘华琳,张瑞,等.食品中甲醛及其检测方法[J].食品工业科技,2013,34(19):373-376.Jin HG,Liu HL,Zhang R,et al.Review of analytical methods for the determination of formaldehyde in food[J].Sci Technol Food Ind,2013,34(19):373-376.
[4]李俊,刘辉,刘嘉,等.乙酰丙酮分光光度法检测果蔬中甲醛含量的改进研究[J].食品科技,2016,41(9):289-294.Li J,Liu H,Liu J,et al.Improvement on acetylacetone spectrophotometry for formaldehyde detection in fruits and vegetables[J].Food Sci Technol,2016,41(9):289-294.
[5]王冬芬,李道敏.乙酰丙酮法测定香菇中的甲醛[J].河南预防医学杂志,2014,25(1):40-42.Wang DF,Li DM.Determination of formaldehyde in mushrooms acetyl acetone method[J].Henan J Prev Med,2014,25(1):40-42.
[6]李俊,吕都,陈中爱,等.果蔬中甲醛提取方法的优选研究[J].食品工业,2017,38(1):32-36.Li J,Lv D,Chen ZA,et al.Optimization research on extract methods of formaldehyde in fruits and vegetables[J].Food Ind,2017,38(1):32-36.
[7]邵仕萍,相大鹏,李华斌,等.乙酰丙酮衍生化高效液相色谱-荧光检测法测定食品中的甲醛[J].食品科学,2015,36(16):241-245.Shao SP,Xiang DP,Li HB,et al.Determination of formaldehyde in foods by high-performance liquid chromatography with fluorescence detection through derivatization with acetylacetone[J].Food Sci,2015,36(16):241-245.
[8]张艳艳,潘小红,张礼红.高效液相色谱法测定食品中甲醛次硫酸氢钠含量[J].食品安全质量检测学报,2017,8(4):1470-1474.Zhang YY,Pan XH,Zhang LH.Determination of sodium formaldehyde sulfoxylate in food by highperformance liquid chromatography[J].J Food Saf Qual,2017,8(4):1470-1474.
[9]甘凝岚,颜春荣,徐春祥.高效液相色谱法测定鸭血制品中甲醛含量[J].食品科学,2014,35(12):204-207.Gan NL,Yan CR,Xu CX.Determination of formaldehyde in duck blood products by HPLC[J].Food Sci,2014,35(12):204-207.
[10]张莉,江丰,范志勇,等.气相色谱-串联质谱联用仪测定大豆及大豆制品中甲醛含量[J].食品研究与开发,2016,37(11):153-156.Zhang L,Jiang F,Fan ZY,et al.Determination of formaldehyde in soybean and soybean product using gas chromatography-tandem mass spectrometry[J].Food Res Dev,2016,37(11):153-156.
[11]唐穂平.柱前衍生高效液相色谱法检测水产品中甲醛的含量[J].食品安全质量检测学报,2016,7(7):2931-2936.Tang SP.Determination of formaldehyde in aquatic products by high performance liquid chromatography with precolumn derivatization[J].JFood Saf Qual,2016,7(7):2931-2936.
[12]孟繁磊,牛红红,宋志峰,等.高效液相色谱法测定黑木耳中甲醛含量[J].食品工业,2017,38(6):311-313.Meng FL,Niu HH,Song ZF,et al.Determination of formaldehyde content in black fungus by HPLC[J].Food Ind,2017,38(6):311-313.
[13]刘瑞芳,廖和菁,胡礼渊,等.高效液相色谱法测定进口鱼柳中的吊白块方法研究[J].食品研究与开发,2016,37(1):164-166.Liu RF,Liao HJ,Hu LY,et al.Study on the determination method of the sodium formaldehyde fulfoxylate in imported fish fillet by HPLC[J].Food Res Dev,2016,37(1):164-166.
[14]DB41/T 424-2005食品中甲醛合次硫酸氢钠(吊白块)的测定[S].DB41/T 424-2005 Determination of sodium formaldehyde sulfoxylate(hanging white block)in food[S].
[15]NY/T 1283-2007香菇中甲醛含量的测定[S].NY/T 1283-2007 Determination of Formaldehyde Content in Lentinula edodes[S].
[16]GB/T 21126-2007小麦粉与大米粉及其制品中甲醛次硫酸氢钠含量的测定[S].GB/T 21126-2007 Determination of sodium formaldehyde suifoxylate in grain products[S].
[17]SC/T 3025-2006水产品中甲醛的测定[S].SC/T 3025-2006 Determination of formaldehyde in aquatic products[S].
[18]魏昭,吴蕊,梁勃,等.2,4-二硝基苯肼衍生化-高效液相色谱法测定面粉中的甲醛[J].食品安全导刊,2016,(11):67-68.Wei Z,Wu R,Liang B,et al.Determination of formaldehyde in flour by high performance liquid chromatography with 2,4-dinitrophenylhydrazine derivatization[J].China Food Saf Magaz,2016,(11):67-68.
[19]吕春华,陈梅,陈笑梅,等.衍生液提取-高效液相色谱法测定食品中甲醛[J].理化检验-化学分册,2011,47(9):1005-1008.Lv CH,Chen M,Chen XM,et al.HPLC determination of formaldehyde in foodstuffs by extraction with derivation solution[J].Ptca(Part B:Chem Anal),2011,47(9):1005-1008.