摘要
目的分析顶空气相色谱-质谱法检测食品中呋喃并对影响因素进行分析,确定最佳的实验条件。方法分析顶空密封加热过程中呋喃和d4-呋喃的泄漏和分解而带来的损失;顶空分析的平衡温度、时间的选择以及加入硫酸铵的作用;比较标准加入法和标准曲线法进行呋喃定量分析结果的差异性。结果顶空分析过程中呋喃和d4-呋喃不会因泄漏和分解而影响其稳定性;选择顶空温度50℃平衡30min,可提高呋喃测定的准确性;加入硫酸铵可提高顶空分析呋喃的灵敏性;标准加入法和标准曲线法是两种等效的定量方法。结论选择d4-呋喃作为内标物,顶空50℃恒温30min后,经气相色谱质谱仪分离扫描,标准曲线法定量,是理想的食品中呋喃检测实验条件。
Ahn To develop a method for determination of ethyl carbamate （EC） in alcoholic beverages using headspace solid-phase micro extraction （HS-SPME） followed by gas chromatography/mass spectrometry. Method After addition of deuterated internal standard ,the optimized HS-SPME extraction with carbowax/divinylbenzene fibres （30min at 70℃ ） was done applying salting out with 2g sodium chloride in the presence of pH 7 buffer solution,inserted into the injection port of the GC/MS for 10 min to accomplish complete desorption,and then analytes were separated by gas chromatography on a DB- WAX capillary column,identified and quantified by mass spectrometry in SIM mode. Results The correlation coefficients were good in the range of 10-1 000μg/L,with a detection limit of 1μg/L and limit of quantity of 10μg/L. EC average recoveries were 88.6-94.7%, and the relative standard deviation（RSD） were in the range of 1.9%-3.6%. Conclusion The method is reliable,rapid and convenient and without the need for any organic solvent,It is a fully automated procedure for determination of ethyl earbamate in alcoholic beverages.
出处
《中国热带医学》
CAS
2010年第10期1224-1225,共2页
China Tropical Medicine
基金
2009年深圳市科技计划项目(200903267)
关键词
呋喃
气相色谱-质谱法
影响因素
食品
Headspaee solid-phase micro extraction （HS-SPME）
Ethyl carbamate
Gas chromatography-mass spectrometry（GC-MS）
Aleoholie beverages.
