| 面制品添加剂偶氮甲酰胺热处理下转化为氨基脲的研究 |
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| 基金项目:广东省科技计划项目（2016A020210012） |
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| 中文摘要:建立了高效液相色谱-串联质谱（HPLC-MS/MS）检测氨基脲（SEM）的方法，并研究了偶氮甲酰胺（ADA）在热处理条件下转化为SEM的规律。该方法以2 硝基苯甲醛为衍生剂，衍生温度为37 ℃，萃取pH值为70。结果表明，SEM在05~100 μg·L-1质量浓度范围内线性关系良好，相关系数（r）为0999，检出限为04 μg·L-1。在10、20、40 μg·L-1加标水平下的回收率为996%~120%，相对标准偏差小于7.6%。实验发现ADA在热处理条件下会降解生成SEM，高温时ADA降解完全；且SEM的生成率随温度升高而增大，在200 ℃时生成率达到最高值0094%，而当温度过高时，SEM会因分解导致生成率下降；烘烤时间过长时（＞30 min），SEM的生成率也会降低。 |
| 中文关键词:高效液相色谱-串联质谱（HPLC-MS/MS） 偶氮甲酰胺 氨基脲 热处理 |
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| Study on Degradation of Flour Additive Azodicarbazide to Semicarbazide under Heat Treatment |
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| Abstract:A method was developed for the determination of semicarbazide（SEM） by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The degradation of azodicarbazide（ADA） to SEM under heat treatment was also studied.The method was optimized by using 2 nitrobenzaldehyde as derivative agent，at a derivative temperature of 37 ℃ and an extraction pH value of 70.The calibration curve was linear in the range of 05-100 μg·L-1 with a correlation coefficient（r） of 0999 and a detection limit of 04 μg·L-1The spiked recoveries at three spiked levels of 10，20 and 40 μg·L-1 were in the range of 996%-120%with relative standard deviations less than 7.6%.Results showed that ADA was degraded into SEM under heat treatment，and it was degraded completely at high temperature.Meanwhile，the formation rate of SEM increased with the increase of temperature，and it reached the maximum value of 0094% at 200 ℃.Nevertheless，the formation rate decreased with the decomposition of SEM when the temperature was exorbitant（>200 ℃）.Besides，it also decreased when the baking time lasted too long（>30 min）. |
| Key Words:high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） azodicarbazide semicarbazide heat treatment |
| 引用本文：黄晓姗，关铭鑫，杭义萍.面制品添加剂偶氮甲酰胺热处理下转化为氨基脲的研究[J].分析测试学报,2018,37(8):977-980. |
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