四-(对甲基苯基)-卟啉柱前衍生-固相萃取富集高效液相色谱法测定烟草中痕量汞  

Determination of Trace Mercury from Tobacco by solid Phase Extraction and High Performance Liquid Chromatography

作　　者：张承明[1] 古昆[2] 王保兴[1] 杨光宇[1] 

机构地区：[1]云南烟草科学研究院烟草化学重点实验室,昆明650106 [2]云南大学应用化学系,昆明650031

出　　处：《云南化工》2002年第3期26-28,共3页Yunnan Chemical Technology

摘　　要：研究了用四 (对甲基苯基 ) 卟啉柱前衍生 ,固相萃取富集 ,高效液相色谱测定烟草中痕量汞的方法。烟草样品用微波消化后 ,用四 (对甲基苯基 ) 卟啉 (T4 MPP)柱前衍生 ,用WatersSep Park C1 8固相萃取小柱萃取富集汞的T4 MPP络合物 ,然后用甲醇 (内含 0 .0 1mol/L四氢吡咯 醋酸缓冲盐 )和四氢呋喃 (内含 0 .0 1mol/L四氢吡咯 醋酸缓冲盐 )梯度洗脱 ,WatersXterraTMRP1 8(3 .9× 15 0mm)色谱柱作为固定相分离 ,用二极管矩阵检测器检测 ,汞含量在 1～ 12 0 μg/L范围内与峰面积成线性关系 ,根据信噪比 (S/N =3 ) ,方法检测限为 0 .3 μg/L ,方法相对标准偏差在 1.5 %～ 2 .4%之间 ,标准回收率在 94%～ 10 6%之间 ,该方法用于测定烟草中的汞 ,结果满意。Trace mercury from tobacco was determined by solid phase extraction and then high performance liquid chromatography. Samples were digested by microwave irradiation firstly, and then pre column derived with tera (4 methylphenyl)porphine(T 4MPP)and extracted with Waters Sep Park C18 cratridge.Mercury chelate was separated on a Waters Xterra TM RP 18 chromatographic column(5μ m,3.9×150),eluted with gradientmethanol THF containing 0.01 mol/L of prolidine acetic acid buffer, and monitored with photodiode array deteceor. The method was satisfactory to determine trace mercury from tobacco with the linear range of mercury in 1～120 μ g/L, detection limit(S/N=3)in 0.3 μ g/L, relative standard deviation in 1.5%～2.4%, and the recovery rate in 94%～106%.

关 键 词：高效液相色谱法 固相萃取 痕量汞 柱前衍生 卟啉 MPP 苯基 甲基苯 矩阵 萃取富集 

分 类 号：TQ231.14[化学工程—有机化工] O65[理学—分析化学]