摘 要:目的:本实验主要研究一种能快速提取、净化茯苓中异丙威并检测其含量的方法。
方法:异丙威是一种氨基甲酸酯类农药。本实验采用高效液相色谱法对异丙威的含量进行测定,选取超声波辅助提取茯苓粉中的异丙威,考察了无水硫酸钠和弗罗里硅土不同比例作固相萃取柱对其净化的影响,不断改变流动相比例以及柱温,比较其对测定的影响,确定了高效液相的色谱条件。
结果:色谱柱(Ultimate XB-C18 5μm 4.6×250mm);柱温:30℃;紫外检测器波长:210nm;进样量:10μl;流动相:乙腈:一级水=55:45(V/V);流速:1.00ml/min;经计算,该方法的回收率为:96.87%,相对标准偏差为:11.65%,实验证明该方法效果好。
关键词:异丙威;高效液相色谱法;茯苓
ABSTRACT:Objective:This paper want to find a fast and accurate method to detect isoprocab from Poria cocos。
Methods:Isoprocarb is a carbamate pesticide。The ultrasonic wave was employed to extract isoprocarb from Poria cocos,the purify condition also been investigated,the contents of isoprocarb was been detected by HPLC。The proportion of Na2SO4 and Florida,which as the solid-phase,was investigated the effect of the compounds which extracted from Poria cocos,the result shown the purification column included 0.4g Na2SO4,1g Florida,0.4g Na2SO4。 The detection method were investigated the column temperature,mobile phase and its proportion,detectin wavelength and velocity for HPLC。The recovery and the loss rate also studied in this paper。
Results:Chromatographic column (Ultimate XB-C18 5μm 4.6×250mm); Column temperature:30℃;Ultraviolet detector wavelength:210nm;Enter the sample weight:10μl;Mobile phase:acetonitrile:level 1 water = 55:45 (V/V);Velocity:1.00 ml/min;The recovery is 96.87%,RSD is 11.65%。This method worked well。
Keywords: Isoprocarb;HPLC;Poria cocos