出口小麦粉及其制品中偶氮甲酰胺的测定
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摘要
建立了面粉及其制品中偶氮甲酰胺的高效液相色谱检测方法。用丙酮旋涡混合提取试样中偶氮甲酰胺,经Syncronis HILIC柱(100 mm×2.1 mm,5μm)在A相:5%甲醇;B相:乙腈;A相∶B相体积比3∶97的条件下洗脱,最佳吸收波长为245 nm。该法灵敏度高,线性关系良好,相关系数r达到0.99,回收率在79.5%～97.5%之间,相对标准偏差(RSD)均小于8%。方法快速、简便、精确度高、准确度高,适用于小麦粉及其制品中偶氮甲酰胺的定性、定量分析。
A high performance liquid chromatography(HPLC) test method was developed for the determination of azodicarbonamide(ADA) in flour and its products. ADA were extracted by acetone vortex mixed, and it was eluted by Syncronis HILIC(100 mm × 2.1 mm, 5 μm) under the conditions of volume ratio of 50 % methanol to acetonitrile 3 ∶ 97, the best absorption wavelength was 245 nm. The method had high sensitivity and good linear relationship, the correlation coefficient reached 0.99, the recovery rate was between 79.5% and 97.5%, and the relative standard deviation(RSD) was less than 8 %. The method was rapid, simple, accurate and accurate. It could be applied to the qualitative and quantitative analysis of wheat flour and its products.
A high performance liquid chromatography(HPLC) test method was developed for the determination of azodicarbonamide(ADA) in flour and its products. ADA were extracted by acetone vortex mixed, and it was eluted by Syncronis HILIC(100 mm × 2.1 mm, 5 μm) under the conditions of volume ratio of 50 % methanol to acetonitrile 3 ∶ 97, the best absorption wavelength was 245 nm. The method had high sensitivity and good linear relationship, the correlation coefficient reached 0.99, the recovery rate was between 79.5% and 97.5%, and the relative standard deviation(RSD) was less than 8 %. The method was rapid, simple, accurate and accurate. It could be applied to the qualitative and quantitative analysis of wheat flour and its products.
引文
[1]陈波,靳保辉,林燕奎,等.面粉中偶氮甲酰胺含量的高效液相色谱法测定[J].分析测试学报,2008,27(9):1002-1004.
[2]周漪波,黄芳,朱志鑫,等.小麦粉中偶氮甲酰胺的高效液相色谱法快速测定[J].食品研究与开发,2010,31(4):102-105.
[3]周陶忆,陆琦,孙凯峰.小麦粉中偶氮甲酰胺检测技术研究[J].现代食品科技,2010,26(12):1412-1414.
[4]叶婧.偶氮甲酰胺、氨基脲检测方法及其在面制品中的变化规律研究[D].石家庄:河北农业大学,2011.
[5]袁丽红,丁洪流,陈英,等.面粉添加剂偶氮甲酰胺代谢物联二脲的HPLC-MS/MS检测[J].分析检测,2013,34(10):73-76.
[6]王雅,王俊苏,向露,等.液相色谱-串联质谱法测定面粉及其制品中的联二脲[J].色谱,2014,32(5):513-518.
[7]MULDER P P J,BEUMER B,VAN RHIJN J A.The determination of biurea:A novel method to discriminate between nitrofurazone and azodicarbonamide use in food products[J].Analytica Chimica Acta,2007,586(1/2):366-373.
[8]TIAN W R,SANG Y X,WANG X H.Semicarbazide-from stateof-the-art analytical methods and exposure to toxicity:A review[J].Food Additives&Contaminants:Part A,2014,31(11):1850-1860.
[9]宋书锋,王丹,刘卿,等.面粉中偶氮甲酰胺的高效液相色谱测定方法的优化[J].中国食品卫生杂志,2014,26(5):448-451.
[10]张桂芳,张晓瑜,宫月华,等.高效液相色谱-紫外检测法快速测定小麦面粉中偶氮甲酰胺[J].中国食品卫生杂志,2014,26(5):473-475.
[2]周漪波,黄芳,朱志鑫,等.小麦粉中偶氮甲酰胺的高效液相色谱法快速测定[J].食品研究与开发,2010,31(4):102-105.
[3]周陶忆,陆琦,孙凯峰.小麦粉中偶氮甲酰胺检测技术研究[J].现代食品科技,2010,26(12):1412-1414.
[4]叶婧.偶氮甲酰胺、氨基脲检测方法及其在面制品中的变化规律研究[D].石家庄:河北农业大学,2011.
[5]袁丽红,丁洪流,陈英,等.面粉添加剂偶氮甲酰胺代谢物联二脲的HPLC-MS/MS检测[J].分析检测,2013,34(10):73-76.
[6]王雅,王俊苏,向露,等.液相色谱-串联质谱法测定面粉及其制品中的联二脲[J].色谱,2014,32(5):513-518.
[7]MULDER P P J,BEUMER B,VAN RHIJN J A.The determination of biurea:A novel method to discriminate between nitrofurazone and azodicarbonamide use in food products[J].Analytica Chimica Acta,2007,586(1/2):366-373.
[8]TIAN W R,SANG Y X,WANG X H.Semicarbazide-from stateof-the-art analytical methods and exposure to toxicity:A review[J].Food Additives&Contaminants:Part A,2014,31(11):1850-1860.
[9]宋书锋,王丹,刘卿,等.面粉中偶氮甲酰胺的高效液相色谱测定方法的优化[J].中国食品卫生杂志,2014,26(5):448-451.
[10]张桂芳,张晓瑜,宫月华,等.高效液相色谱-紫外检测法快速测定小麦面粉中偶氮甲酰胺[J].中国食品卫生杂志,2014,26(5):473-475.