过硫酸钾存在下极谱催化波法测定芬布芬

Determination of Fenbufen Based on Its Polarographic Catalytic Wave in the Presence of Persulfate

研究了芬布芬（Fenbufen,FBF）在K2S2O8存在下的极谱催化波。在0.2 mol/L HAc-NaAc（pH=5.0）缓冲溶液中,FBF的羰基于EP=-1.18 V（vs.SCE）处产生了不可逆的还原波。K2S2O8存在时,该羰基还原中间产物被过硫酸根氧化在原电位处产生了FBF的平行催化波。该平行催化波比相应的还原波分析灵敏度提高了10倍,峰电流与FBF浓度在7.08×10^-6-2.36×10^-5mol/L（r=0.993 1,n=7）和2.36×10^-8-7.08×10^-6mol/L（r=0.998 9,n=8）范围内呈良好线性关系;检出限为7.78×10^-9mol/L（3σ）。11次平行测定4.72×10^-7mol/L FBF,相对标准偏差RSD为1.2%。可用于原料药、片剂、胶囊等制剂中FBF含量的测定。

A catalytic polarographic determination of fenbufen （FBF） in the presence of K2 S208 was described. In 0.2 mol/L HAc-NaAc（pH = 5.0） buffer, the polarographic reduction of carbonyl group of FBF yielded an irreversible reduction wave at a peak potential Ep of - 1.18 V（vs. SCE）. When 4 × 10^-4 mol/L K2S2O8 was present in the buffer, the reduced FBF intermediate was oxidized by persulfate, producing a catalytic wave at the original potential. The analytical sensitivity of the catalytic wave was 10 times higher than that of the corresponding reduction wave. The peak current of the catalytic wave varied linearly with the FBF concentration over the range from 7.08 × 10^-6 mol/L to 2. 36 × 10^-5 mol/L（ r = 0. 993 1, n = 7 ） and from 2. 36 × 10^-8 mol/L to 7.08 × 10^-6 mol/L（r =0. 998 9, n =8） with a detection limit of 7.78 × 10^-9 mol/L （3σ）. RSD（ n = 11 ） was 1.2% at the concentration level of 4.72 × 10^ -7 mol/L. The proposed method was applied to the determination of FBF in the raw material, in tablets and in capsules without previous treatment.