| 柱前衍生/高效液相色谱法测定烟用添加剂中的咪唑 |
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| 基金项目:中烟实业科技项目（ZYSY2012-06） |
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| 中文摘要:建立了丹磺酰氯柱前衍生/高效液相色谱（HPLC）测定烟用添加剂中咪唑含量的分析方法。添加剂样品经碳酸盐缓冲溶液处理，丹磺酰氯进行柱前衍生化后，再经乙酸乙酯萃取，取有机层萃取液经干燥、过滤、浓缩、乙腈定容、过滤后，以C18柱为色谱柱，乙腈-水为流动相梯度洗脱，荧光检测器检测。确定最佳的衍生化反应条件为：丹磺酰氯溶液质量浓度1 000 mg/L，反应温度45 ℃，缓冲溶液pH值10.0，超声振荡反应时间40 min,咪唑衍生物用外标法进行定量分析。该方法在0.5~500 mg/L范围内线性关系良好，相关系数（r）为0.999 5，对咪唑的检出限为0.24 mg/kg，定量下限为0.80 mg/kg，0.5、10.0、500 mg/L 3个加标水平下的回收率为89.1%~97.2%，相对标准偏差不大于7.5%。该方法准确可靠，适用于烟用添加剂中咪唑含量的测定。 |
| 中文关键词:柱前衍生 高效液相色谱（HPLC） 烟用添加剂 咪唑 丹磺酰氯 |
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| Determination of Imidazole in Cigarette Additives by High Performance Liquid Chromatography with Pre-column Derivatization |
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| Abstract:An effective method of high-performance liquid chromatography（HPLC）was developed for the determination of imidazole，the harmful ingredient in cigarette additives based on pre-column derivatization with dansyl chloride（Dns-Cl）.The additive samples firstly underwent the treatment of a buffer of carbonate solution，followed by the pre-column derivatization with dansyl chloride，then the extraction with ethyl acetate，dryness，evaporation，dilution with acetonitrile and filteration，separation on a C18 column，elution with acetonitrile-water by gradient elation，and finally the detection with a fluorescence detector.The optimum derivatising conditions of imidazole with dansyl chloride are as follows:concentration of dansyl chloride:1 000 mg/L;temperature of reaction:45 ℃;pH of buffer solution:10.0;time of reaction:40 min.
The imidazole derivative was quantified by the external standard method.There was a good linearity for the analyte in the range of 0.5-500 mg/L with a correlation coefficient of 0.999 5.The limits of detection of the method for imidazole derivative was 0.24 mg/kg，and the limits of quantitation was 0.80 mg/kg.The recoveries at three spiked levels ranged from 89.1% to 97.2% with RSDs not more than 7.5%.Results showed that the method was accurate and reliable，and was applicable to the determination of imidazole content in cigarette additives. |
| Key Words:pre-column derivatization high-performance liquid chromatography（HPLC） cigarette additives imidazole dansyl chloride |
| 引用本文：程利侠，何东香，杨金龙，吕长平.柱前衍生/高效液相色谱法测定烟用添加剂中的咪唑[J].分析测试学报,2018,37(9):1056-1060. |
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