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目的:确定以Ce(Ⅳ)直接氧化化学发光法分析测定头抱类β-内酰胺抗生素的新方法。方法:由于β-内酰胺抗生素水解一般都生成含有巯基(-SH)的化合物,用Ce(Ⅳ)直接氧化含巯基(-SH)的化合物能产生弱发光,且Rh6G能大大增强此弱发光,由此建立了测定头孢拉定等5种头抱类β-内酰胺类抗生素的FIA-CL分析法。结果:在选定的最佳条件下,经测试5个头孢类抗生素浓度在1.0×10~(-8)～1.5×10~(-5)g·mL~(-1)范围内与化学发光强度呈良好的线性关系。对5.0×10~(-6)g·mL~(-1)的头孢试样进行11次平行测定,得到RSD对头孢拉定、头孢呋辛钠、头孢噻肟钠、头孢曲松钠、头孢哌酮钠分别为2.2％,2.5％,2.7％,2.8％,2.8％。其检出限(3σ)对5个头孢类抗生素顺次分别为3.0×10~(-8),3.5×10~(-8),3.8×10~(-8),3.9×10~(-8),4.0×10~(-8),4.0×10~(-8)g·mL~(-1)。结论:本方法快捷、简便且具有较高的灵敏度,本法用于头孢合成样品的分析,结果满意。
OBJECTIVE: To determine a new method for the determination of head-bound β-lactam antibiotics by Ce (Ⅳ) direct oxidation chemiluminescence. Methods: Compounds containing mercapto (-SH) were generally produced by the hydrolysis of β-lactam antibiotics. The direct oxidation of thiol (-SH) containing compounds with Ce (Ⅳ) produced weak luminescence and Rh6G enhanced the weak luminescence. Thus, a FIA-CL assay for the determination of 5 cephalosporins such as cefradine has been established. Results: Under the optimal conditions, the concentration of 5 cephalosporins tested was in the range of 1.0 × 10 -8 ~ 1.5 × 10 -5 g · mL -1 with chemiluminescence Intensity showed a good linear relationship. The determination of cefradizime, cefuroxime sodium, cefotaxime sodium, ceftriaxone sodium and cefoperazone sodium were carried out on 11 replicates of 5.0 × 10 ~ (-6) g · mL ~ (-1) 2.2%, 2.5%, 2.7%, 2.8%, 2.8%. The limits of detection (3σ) of 5 cephalosporins were 3.0 × 10 -8, 3.5 × 10 -8, 3.8 × 10 -8, 3.9 × 10 ~ (- 4.0 × 10 ~ (-8), 4.0 × 10 ~ (-8) g · mL ~ (-1). Conclusion: The method is fast, simple and has high sensitivity. The method is applied to the analysis of cephalosporin synthetic samples with satisfactory results.