香烟中氨含量的优化离子色谱测定法  被引量:2

Determination of Ammonia in Cigarette Using Optimized Ion Chromatography Method

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作  者:李伟青[1] 张峰[1] 张元[1,2] 袁飞[1] 艾小勇[1,3] 

机构地区:[1]中国检验检疫科学研究院,北京100123 [2]中国医科大学,沈阳110001 [3]华中农业大学,武汉430070

出  处:《食品工业》2015年第6期276-278,共3页The Food Industry

基  金:质检公益行业专项(201310134);质检公益行业专项(201410088);中国检验检疫科学研究院基科研业务费"分子生物学在转基因烟草检测控制中的应用研究"(2013JK018)

摘  要:建立了香烟中氨含量的离子色谱(IC)快速测定方法。样品采用稀硫酸(0.012 5 mol/L)超声提取30 min,离心(10 000 r/min,10 min),上清液经石墨化炭黑柱(GCB)净化提取后采用离子色谱进行分析。以甲基磺酸(0.02mol/L)为淋洗液,采用Dionex Ion PacTM CS12A阳离子交换柱分离,NH4+在质量浓度范围0.5~50 mg/L内二次回归系数良好(r2=0.999 5),检出限(LOD)为0.001 6 mg/g,定量限(LOQ)为0.004 5 mg/g,采用低、中、高3个添加水平,平行测定6次,所得平均回收率分别为90.3%、89.6%和92.5%,相对标准偏差(RSD)分别为4.1%、2.8%和3.3%。A method based on ion chromatography (IC) was established for the detennination of ammonia in cigarette. The cigarette sample was ultrasonic extracted with 0.012 5 mol/L H2SO4. After the ultrasonic treatment, samples were centrifuged (10 000 r/min, 10 min) to obtain the supematant. And then the supematant was cleaned up using GCB solid phase extraction prior to ion chromatographic analysis using DionexlonPacTM CS 12A cation exchange column with methane sulfonic acid (0.02 mol/L) as eluent. The good quadratic regression coefficient (r2=0.999 5) was achieved for the compound over the range of 0.5-50 mg/L. The limits of detennination (LOD) and limits of quanlitation (LOQ) were 0.001 6 mg/g and 0.004 5 mg/g, respectively. The recoveries for the compound in cigarette were 90.3%, 89.6% and 92.5% at the three fortified levels. The relative standard deviations (RSD) of the three fortified levels for the compound were 4.1%, 2.8% and 33%.

关 键 词:香烟  固相萃取 离子色谱 

分 类 号:TS47[农业科学—烟草工业]

 

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