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间接极谱法和阴极溶出伏安法测定头孢克洛的碱性降解产物。

Indirect polarographic and cathodic stripping voltammetric determination of cefaclor as an alkaline degradation product.

作者信息

Rodrigues L N, Zanoni M V, Fogg A G

机构信息

Departamento de Química Analítica, Instituto de Química, Araraquara SP, Brazil.

出版信息

J Pharm Biomed Anal. 1999 Nov;21(3):497-505. doi: 10.1016/s0731-7085(99)00174-0.

Abstract

Cefaclor is not reducible at a mercury electrode, but it can be determined polarographically and by cathodic stripping voltammetry as its initial alkaline degradation product which is obtained in high yield by hydrolysis of cefaclor in Britton-Robinson (B-R) buffer pH 10 at 50 degrees C for 30 min (reduction peak at pH 10, -0.70 V). Differential pulse polarographic calibration graphs are linear up to at least 1 x 10(-4) mol/l(-1). Recoveries of 93% of the cefaclor (n = 3) were obtained from urine spiked with 38.6 microg/ml(-1) using this polarographic method with 1 ml urine made up to 10 ml with pH 10 buffer. Using cathodic stripping voltammetry and accumulating at a hanging mercury drop electrode at - 0.2 V for 30 s, linear calibration graphs were obtained from 0.35 to 40 microg/ml(-1) cefaclor in B-R buffer pH 10. A relative standard deviation of 4.2% (eta = 5) was obtained, and the limit of detection was calculated to be 2.9 ng/ml(-1). Direct determination of cefaclor in human urine (1 ml of urine was made up to 10 ml with pH 10 buffer) spiked to 0.39 microg/ml(-1) was made (recovery 98.6%).

摘要

头孢克洛在汞电极上不可还原,但可通过极谱法和阴极溶出伏安法测定,其初始碱性降解产物可通过在50℃的pH 10 Britton-Robinson(B-R)缓冲液中水解头孢克洛30分钟高产率获得(在pH 10时的还原峰,-0.70 V)。微分脉冲极谱校准曲线在至少1×10⁻⁴mol/L⁻¹范围内呈线性。使用这种极谱法,从添加了38.6μg/ml⁻¹的尿液中回收了93%的头孢克洛(n = 3),将1 ml尿液用pH 10缓冲液稀释至10 ml。使用阴极溶出伏安法并在悬汞滴电极上于-0.2 V处富集30 s,在pH 10的B-R缓冲液中,头孢克洛浓度从0.35至40μg/ml⁻¹获得线性校准曲线。相对标准偏差为4.2%(η = 5),检测限计算为2.9 ng/ml⁻¹。直接测定添加至0.39μg/ml⁻¹的人尿液(1 ml尿液用pH 10缓冲液稀释至10 ml)中的头孢克洛(回收率98.6%)。

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