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高效液相色谱法测定卷烟爆珠中的甲醛与乙醛
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作者单位
刘欣,田丽梅,杨叶昆,黄海涛,缪恩铭,王晋,许永,向明,李晶 云南中烟工业有限责任公司技术中心 
基金项目:中国烟草总公司标准预研项目(2016QB007)
中文摘要:基于自主设计的一种新型的集萃取、过滤和转移功能为一体的样品萃取管,建立了高效液相色谱(HPLC)测定卷烟爆珠中甲醛和乙醛的分析方法。爆珠用乙腈水溶液萃取,在酸性条件下,经2,4 二硝基苯肼衍生化后,衍生物直接用HPLC法测定。结果表明:采用改进的样品萃取管可大大简化前处理步骤,甲醛和乙醛分别在8~1 500 μg/L与10~1 650 μg/L范围内呈较好的线性关系,相关系数(r2)大于0999,检出限分别为25、28 μg/L,定量下限分别为80、95 μg/L;在20、50、100 μg/g 3个加标水平下的平均回收率为969%~1011%,日内精密度和日间精密度均小于4%。该方法具有较好的重复性,适用于卷烟爆珠中甲醛和乙醛的测定。
中文关键词:卷烟爆珠  甲醛  乙醛  萃取  高效液相色谱法(HPLC)
 
Determination of Formaldehyde and Acetaldehyde in Cigarette Capsules by High Performance Liquid Chromatography
Abstract:A high performance liquid chromatographic(HPLC) method was established for the analysis of formaldehyde and acetaldehyde in cigarette capsules based on a novel extraction tube device integrating extraction,filtering and transfer in one step.The cigarette capsules were extracted with aqueous solution of acetonitrile(50% by volume) for 25 min.After purification,the extracts were allowed to derivatively react with 2,4 dinitrophenylhydrazine in an acidic condition(pH 48).Then the derivatives of the extracts were analyzed by HPLC.The results indicated that the extraction tube device greatly simplified the sample preparation for HPLC analysis.Furthermore,the formaldehyde and acetaldehyde in the capsules were successfully separated and determined.The calibration curves for them both were linear in the ranges of 8-1 500 μg/L and 10-1 650 μg/L,respectively,with their correlation coefficients(r2) larger than 0999.The limits of detection(LOD) and quantitation(LOQ) for formaldehyde and acetaldehyde were 25 μg/L and 28 μg/L,and 80 μg/L and 95 μg/L,respectively.The mean recoveries for the target compounds were in the range of 969%-1011% with the intra day and inter day precisions both below 4%.The method provides a new strategy for the quantitation on formaldehyde and acetaldehyde in cigarette capsules with unprecedented simplicity,high precision and great reproducibility.
Key Words:capsule of cigarette  formaldehyde  acetaldehyde  extraction  high performance liquid chromatography(HPLC)
引用本文:刘欣,田丽梅,杨叶昆,黄海涛,缪恩铭,王晋,许永,向明,李晶.高效液相色谱法测定卷烟爆珠中的甲醛与乙醛[J].分析测试学报,2018,37(7):810-814.
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