高效液相色谱法测定棉秆水解液中苯酚和糠醛

HPLC Determination of Phenol and Furfural in Hydrolysate of Cotton Stalks

取经折断并粉碎至大小约为0.63mm的棉秆样品,用硫酸(2.7+97.3)溶液在110℃水解4h,用0.45μm滤膜过滤。采用Shim-pack VP-ODS C18色谱柱及甲醇-水(70+30)溶液作流动相进行分离,并用PDA于272nm作紫外检测及高效液相色谱外标法定量测定棉秆水解产物中的苯酚和糠醛含量。苯酚在0.01～20.0mg.L-1范围内呈线性关系,糠醛在0.01～30.0mg.L-1范围内呈线性关系。苯酚和糠醛的检出限(3S/N)均为0.005mg.L-1。苯酚和糠醛分别在3个浓度水平上做回收率试验,测得回收率分别为90.6%～100.5%和92.9%～99.8%。测定值的相对标准偏差(n=6)分别在1.1%～2.1%和1.7%～2.5%范围内。

Cotton stalks were snapped and crushed to size of ca. 0.63 mm and hydrolyzed in H2SO4 （2. 7＋ 97.3） solution at 110 ℃ for 4 h. After cooling and centrifuging, the supernatant was taken and filtered on 0. 45μm filtering membrane. The filtrate was used for HPLC analysis for phenol and furfural, using Shim-pack VP-ODS Q8 column and mobile phase of CH3OH-H2O （70＋30） for separation and UV-detection with PDA detector at 272 nm for determination of both the phenol and furfural in the linearity ranges of 0. 01 to 20. 0 mg · L^-1 and 0. 01 to 30. 0 mg · L^-1 respectively. Detection limits （3S/N） found were same as 0. 005 mg · L^-1. Values of recovery found, by addition of standards at 3 concentration levels, were in the ranges of 90. 6%- 100. 5% and 92. 9%- 99.8% with values of RSD＇s （n=6） in the ranges of 1.1%-2. 1% and 1. 7% -2. 5% for phenol and furfural respectively.