摘要
建立了同时测定烟用添加剂中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚的高效液相色谱检测方法。样品经稀释剂稀释、振荡、过滤后，采用Thermo Scientific C18（4．6i．d ×250mm，5μm）柱，以y（乙腈）：v（0．1％甲酸水溶液）=33：67为流动相，在流速1．0mL／min条件下等度洗脱分离，在波长为273nm下以二极管阵列检测器检测，以外标法定量。结果表明，9min内即可实现4种目标物的分离，香兰素、乙基香兰素、麦芽酚和乙基麦芽酚的线性范围分别为0．0139～264．5mg!kg，0．0554—302．7mg／kg，4．01～262．9mg／kg和2．32—258．1mg／kg；线性相关系数分别为0．9998，0．9999，0．9999和0．9997；检出限（S／N=3）分别为0．00349，0．00554，1．29和0．58mg/kg；添加水平为10．75—59．14mg／kg时，加标回收率为96．8％～102．2％，相对标准偏差为0．62％-1．6％。方法适用于烟用添加剂中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚的含量检测。
High performance liquid chromatographic method for simultaneous determination of vanillin, ethyl- vanillin, maltol and ethylmaltol in cigarette additives was established. After diluted, vibration and filtration, the cigarette additives were separated on a Thermo Scientific C18（4.6 i. d × 250 mm, 5 μm） column in isocratic elution mode using acetonitrile ： 0. 1% formic acid （ 33 ： 67, V/V） as the mobile phase at 1.0 mL/min. The quantification of these cigarette additives was achieved with external standard method on a diode - array detector at 273 nm. Baseline separation of vanillin, ethyl-vanillin, maltol and ethylmaltol was achieved within 9 min. The linear ranges for vanillin, ethyl-vanillin, mahol and ethylmahol were 0. 0139 - 264.5 mg/kg, 0. 0554 302.7 mg/kg, 4.01 - 262.9 mg/kg and 2.32 ~ 258.1 mg/kg, respectively. The linear correlation coefficients for vanillin, ethyl-vanillin, maltol and ethylmaltol were 0. 9998, 0. 9999, 0. 9999 and 0. 9997, respectively. The detection limits （ S/N = 3 ） for vanillin, ethyl-vanillin, maltol and ethylmaltol were 0. 00349, 0. 00554, 1.29, and 0. 58 mg/kg, respectively. The recoveries and the relative standard deviations （ RSD, n = 9 ） at the spiked concentration of 10. 75 -59. 14 mg/kg were 96. 8% - 102.2% and 0. 62% - 1.6% , respectively. The proposed method has the merits of easy operation, short analysis time and accurate results, which is very suitable for the simultaneous determination of vanillin, ethyl-vanillin, maltol and ethylmaltol in cizarette additives.
出处
《分析试验室》
CAS
CSCD
北大核心
2014年第8期950-954,共5页
Chinese Journal of Analysis Laboratory
