摘要
用固相萃取-高效液相色谱-二极管阵列检测法建立了测定烟草中两种多羟基吡嗪异构体的方法。烟草中的2-（1′,2′,3′,4′-四羟基丁基）-5-（2″,3″,4″-三羟基丁基）-吡嗪（2,5-DOF）和2-（1′,2′,3′,4′-四羟基丁基）-6-（2″,3″,4″-三羟基丁基）-吡嗪（2,6-DOF）用甲醇索氏萃取2h后,提取液用Waters Sep-Park-C18固相萃取小柱预分离,选择Waters carbohydrate analysis（3.9 mm×300 mm）色谱柱（NH2柱）,V（乙腈）∶V（水）=80∶20为流动相,流速：1.0 mL/min,烟草中的2,5-DOF及2,6-DOF达到基线分离。两种异构体的标准曲线的线性回归系数均大于0.9996,线性范围为0.5-100μg/mL;标准回收率分别为98%和104%;相对标准偏差均小于3%;检出限为0.2μg/mL。用该方法测定了不同卷烟中的2,6-DOF和2,5-DOF两种异构体。
Solid phase extraction-high performance liquid chromatography-DAD method has been developed for the de- termination of 2-（ 1＇, 2＇, 3＇, 4＇-tetrahydroxy-butyl）-5-（2＂, Y＇, 4＂-trihydroxy-butyl）-pyrazine （2,5-DOF） and 2-（ 1＇, 2＇, 3＇, 4＇-tetrahydroxy - butyl） -6- （2＂, Y＇, 4＂-trihydroxy-butyl ） -pyrazine （2,6-DOF） in tobacco. The 2,5 - DOF and 2,6- DOF were separated from tobacco samples by Soxhlet Methanol Extraction, and then cleaned up by solid phase extraction on a waters Sep-Pak-C18 cartridge. The DOFs were separated on a Carbohydrate Analysis column （3.9 mm ×300 mm）＂. The mobile phase was acetonitrile-water （80：20, V/V） at a flow rate of 1 mL/min. Each DOF was monitored by photodiode array detector at its maximum absorption wave-length. There were good linear correlations between the peak areas and concentrations of the DOFs （the correlation coefficients are above 0.9996）. The linear range is 0.5 100 μg/mL for the DOFs. The recovery of the DOFs were 98% and 104%. The relative standard deviation was not more than 3 %. The detection limit is 0.2 μg/mL. This method was applied to the determination of the DOFs in tobacco with good results.
出处
《分析试验室》
CAS
CSCD
北大核心
2007年第12期35-38,共4页
Chinese Journal of Analysis Laboratory
关键词
高效液相色谱
固相萃取
2-(1′
2′
3′
4′-四羟基丁基)-5-(2″
3″
4″-三羟基丁基)-吡嗪
2-(1′
2′
3′
4′-四羟基丁基)-6-(2″
3″
4″-三羟基丁基)-吡嗪
烟草
High performance liquid chromatography
Solid phase extraction
2- （ 1＇, 2＇, 3＇, 4＇-tetrahydroxy-butyl） -5 - （2＂, Y＇, 4＂-trihydroxy-butyl ）-pyrazine
2- （ 1＇, 2＇, 3＇, 4＇-tetrahydroxy-butyl ）-6- （ 2＂, 3＂, 4＂-trihydroxy-butyl）-pyrazine
Tobacco
