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作 者:李响丽[1,2] 李国智 范多青 杨仁礼 毛多斌[1]
机构地区:[1]郑州轻工业学院食品与生物工程学院,河南郑州450002 [2]红云红河(烟草)集团技术中心,云南昆明650202
出 处:《分析测试学报》2012年第1期56-61,共6页Journal of Instrumental Analysis
基 金:云南中烟科技项目资助(2011JC07)
摘 要:建立了超高效液相色谱(UPLC)对卷烟主流烟气总粒相物中甲醛、乙醛、丙酮、巴豆醛等8种羰基化合物的测定方法。采用经2,4-二硝基苯肼酸性溶液处理过的剑桥滤片捕集烟气,再用含2%(体积分数)吡啶的乙腈溶液进行萃取,以KinetexTM C18(150 mm×2.1 mm,2.6μm)为色谱柱,水-乙腈(35∶65)和水-乙腈-四氢呋喃-异丙醇(59∶30∶10∶1)为流动相梯度洗脱,采用二极管阵列检测器进行检测,分析时间为20 min。结果表明,该方法的相关系数r2≥0.999 97,检出限为25.81~67.74 ng/cig,平均加标回收率为95%~99%,相对标准偏差为1.4%~5.8%。各组分峰分离度高、分析时间短、流动相耗量少、结果准确可靠。用该方法对20种不同卷烟牌号样品中8种羰基化合物的含量进行测定,结果满意。An Ultra Performance Liquid Chromatographic(UPLC) method was developed for the separation and determination of formaldehyde,acetaldehyde,acetone,acrolein,propionaldehyde,crotonaldehyde,2-butanone,butyraldehyde in cigarette mainstream smoke.The targeted compounds in cigarette mainstream smoke were collected with a Cambridge fliter treated with acidic solution of 2,4-dinitrophenylhydrazine,and extracted with 50 mL 2% pyridine acetonitrile.The carbonyl compounds were separated on a KinetexTM C18(150 mm×2.1 mm,2.6 μm) column,using water-acetonitrile(35 ∶65) mixed solution and water-acetonitrile-tetrahydrofuran-isopropyl alcohol(59 ∶30 ∶10 ∶1) as mobile phases by gradient elution.The eight carbonyl compounds were separated in 20 min and determined by UPLC with a diode array detector.The result indicated that the correlation coefficients(r2) of eight carbonyl compounds were not less than 0.999 97.The detection limits for the method were between 25.81 ng/cig and 67.74 ng/cig.The average recoveries were in the range of 95%-99% with relative standard deviations of 1.4%-5.8%.Compared with the YC/T 254-2008 standard method,the proposed method was faster,simpler and less consumption,and was applied in the determination of eight carbonyl compounds in twenty kinds of cigarette with satisfactory results.
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