Emerson试剂分光光度法测定头孢羟氨苄
Spectrophotometric Determination of Cefadroxil with Emerson Reagent
摘 要
采用Emerson试剂分光光度法测定头孢羟氨苄的含量。在pH 9.60的四硼酸钠-氢氧化钠缓冲溶液中,在铁氰化钾存在下,头孢羟氨苄可与4-氨基安替比林发生反应,生成红色的化合物,组成比为1比1,最大吸收波长为508 nm。头孢羟氨苄的质量浓度在1.20~110.0 mg·L-1范围内与其吸光度呈线性关系,方法的检出限(3s/k)为0.80 mg·L-1。方法应用于头孢羟氨苄胶囊中头孢羟氨苄含量的测定,测定结果与药典法测定值相符,测定值的相对标准偏差(n=5)在0.20%~0.71%之间。Emerson试剂与头孢羟氨苄的反应机理被初步探讨。
Emerson试剂
头孢羟氨苄
4-氨基安替比林
Spectrophotometry
Emerson reagent
Cefadroxil
4-Aminoantipyrine
Abstract
Spectrophotometry was applied to the determination of cefadroxil with emerson reagent. In Na2B4O7-NaOH buffer solution of pH 9.60, a red compound was produced by the reaction of cefadroxil with 4-aminoantipyrine in the presence of K3Fe(CN)6. The stoichiometric ratio of the compound was 1∶1 and the maximum absorption wavelength found was 508 nm. Linear relationship between values of absorbance and mass concentration of cefadroxil was obtained in the range of 1.20-110.0 mg·L-1, with detection limit (3s/k) of 0.80 mg·L-1. The proposed method was applied to the analysis of drug samples of cefadroxil, giving results in consistency with the values obtained by pharmacopoeia method with RSD′s (n=5)in the range of 0.20%-0.71%. Reaction mechanism of Emerson reagent and cefadroxil was also studied preliminarily.
中图分类号 O657.32
所属栏目 工作简报
基金项目
收稿日期 2013/9/3
修改稿日期
网络出版日期
作者单位点击查看
联系人作者潘自红(zhpan80@163.com)
备注潘自红(1980-),女,河南信阳人,讲师,硕士,研究方向为光分析。
引用该论文: PAN Zi-hong,LI Qing-bin,ZHAO Xiao-jun,HOU Yan-min,CAO Ai-juan. Spectrophotometric Determination of Cefadroxil with Emerson Reagent[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(9): 1142～1145
潘自红,李青彬,赵晓军,侯延民,曹爱娟. Emerson试剂分光光度法测定头孢羟氨苄[J]. 理化检验－化学分册, 2014, 50(9): 1142～1145
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参考文献
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【2】SALEM H. Selective spectrophotometric determination of phenolic β-lactam antibiotics in pure forms and in their pharmaceutical formulations［J］. Anal Chim Acta, 2004,515(2):333-341．
【3】SALEM H, SALEH G A. Selective spectrophotometric determination of phenolic β-lactam antibiotics［J］. J Pharmaceu Biomed Anal, 2002,28(6):1205-1213．
【4】SHARIF S, KHAN I U, ASHFAQ M, et al. Development and validation of a high performance liquid chromatographic method for the simultaneous determination of potassium clavulanate and cefadroxil in synthetically prepared tablets［J］. J Anal Chem, 2010,65(10):1029-1034．
【5】蔡玉娥,蔡亚岐,牟世芬,等.高效液相色谱-紫外光度法检测尿液和牛奶中多种头孢类抗生素［J］.分析化学, 2006,34(6):745-748．
【6】刘一鸣,宣春生,李文英,等.荧光猝灭法对头孢羟氨苄和头孢拉定荷移反应研究［J］.光谱学与光谱分析, 2009,29(2):441-445．
【7】TOMITA I N, BULHES L O S. Electrogenerated chemiluminescence determination of cefadroxil antibiotic［J］. Anal Chim Acta, 2001,442(2):201-206．
【8】MOLINA-GARCIA L, LLORENT-MARTINEZ E J, FERNANDEZDE CORDOVA M L F, et al. Direct determination of cefadroxil by chemiluminescence using a multicommutated flow-through sensor［J］. Spectroscopy Letters: An International Journal for Rapid Communication, 2010,43(1):60-67．
【9】FENG Su-ling, JIANG Ju-hui, FAN Jing, et al. Sequential injection analysis with spectrophotometric detection of cefadroxil and amoxicillin in pharmaceuticals［J］. Chem Anal, 2007,52(1):83-92．
【10】THONGPOON C, LIAWRUANGRATH B, LIAWRUANGRATH S, et al. Flow injection chemiluminescence determination of cefadroxil using potassium permanganate and formaldehyde system［J］. J Pharmaceu Biomed Anal, 2006,42(2):277-282．
【11】HU Sheng-zhi, BAREON R J, JOHNSON K E, et al. The structure research of the reaction product between 4-aminoantipyrine and phenol［J］. Nature, 1985,9(1):78-79．
【12】中华人民共和国药典委员会.中华人民共和国药典(二部)［M］.北京:化学工业出版社, 2005:153-155．
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