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