气相色谱-质谱法测定浓缩苹果汁中丁酰肼残留量
GC-MS DETERMINATION OF RESIDUAL DAMINOZIDE IN APPLE JUICE CONCENTRATE
摘 要
采用在碱性条件下将样品中丁酰肼水解为不对称二甲基联氨,再用水杨醛与之发生衍生化反应的前处理方法,建立了浓缩苹果汁中丁酰肼残留量的气相色谱-质谱(GC-MS)测定方法.以丁酰肼浓度对峰面积作图得校正曲线,回归方程为y=100 211 x-11 156(r=0.999 6),检出限(3S/N)为0.01 mg·kg-1,测定结果的相对标准偏差为1.60%~6.23%,回收率为92%~107%.
浓缩苹果汁
丁酰肼残留量
GC-MS
Apple juice concentrate
Daminozide
Abstract
In the GC-MS method described,daminozide was hydrolyzed,in the presence of a strong base,to for unsymmetrical dimethylhydrazine,which was then distilled from the apple juice matrix,and derivatized with salicylaldehyde to form salicylaldehyde dimethylhydrazone.The derivatized product was determined by GC-MS using selected ion monitoring mode.The calibration curve was obtained by plotting the peak area against the concentration of daminozide giving the linear regression equation,y=100 211 x-11 156 (r=0.999 6) and a detection limit (3S/N) of 0.01 mg·kg-1.Tests for precision and recovery of this method gave results of RSD′s in the range of 1.60% to 6.23%,and average recoveries in the range from 92% to 107%.
中图分类号 O657.37
所属栏目 工作简报
基金项目
收稿日期 2005/5/10
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备注孔祥虹(1965-),男,宁夏银川市人,硕士,高级工程师,主要从事食品、农产品检验工作.
引用该论文: KONG Xiang-hong,TANG Hua,LI Jian-hua,HE Xue-wen. GC-MS DETERMINATION OF RESIDUAL DAMINOZIDE IN APPLE JUICE CONCENTRATE[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(9): 721～722
孔祥虹,汤桦,李建华,何学文. 气相色谱-质谱法测定浓缩苹果汁中丁酰肼残留量[J]. 理化检验－化学分册, 2006, 42(9): 721～722
被引情况:
【1】曹晔,王力,韩卓珍,张光友,刘建国, "气相色谱-质谱法测定大气中偏二甲肼",理化检验－化学分册 46, 1184-1186(2010)
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参考文献
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【2】Chevrier J P,Pfister A.Toxicity of 1,1-dimethylhydrazine in animals Ⅱ chromic roisoning[J]. Eur J Toxicol,1974,7:242．
【3】Hans G J,Mol,Ruud C J,Van Dam.Determination of daminozide in apple and apple leaves by liquid chromatography-mass spectrometry[J].J Chromatogr A,1999,833:53．
【4】Jan H W,Anton G,Van D.Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorus detection[J].J Chromatogr A,1996,723:355．
【5】Marcel A R,Hans R B.Determination of daminozide and dimethylhydrazine residues in swiss apple juice concentrates using gas chromatography-mass spectrometry[J].J Agric Food Chem,1991,39:176．
【6】林黎明.超声衍生化GC-MS检测花生中丁酰肼残留[J].化学通报,2000,11:300．
【7】李秀勇,阮新.花生中丁酰肼残留量的气相色谱法测定[J].分析测试技术与仪器,2000,6(4):232．
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