Sun Han-wen, Wu Yuan-yuan, Li Li-qing
College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China.
Drug Test Anal. 2009 Mar;1(3):128-34. doi: 10.1002/dta.25.
A novel trivalence dysprosium(Dy(3+))-sensitized chemiluminescence method was developed for the first time for the determination of enoxacin (ENX) using flow-injection sampling based on the chemiluminescence (CL) associated with the reaction of the Dy(3+)-cerium(Ce(IV))-S(2)O(3) (2-)-ENX system and the Dy(3+)-MnO(4) (-) S(2)O(3) (2-)-ENX system. The analytical conditions for CL emission were investigated and optimized. The relationship between the CL intensity of ENX and its concentration has good linearity, with a correlation coefficient of 0.9984-0.9994. The limit of detection (LOD, 3sigma) was 0.20 ng/mL for the Dy(3+)-ENX-S(2)O(3)(2-)-Ce(IV)-H(2)SO(4) system and 0.22 ng/mL for the Dy(3+)-ENX-S(2)O(3)(2-)-MnO(4) (-)-HNO(3) system. The relative standard deviation (RSD, n = 11) was 1.8% for 11 determinations of 60 ng/mL ENX. The proposed method was applied to the analysis of ENX in injections, serum and urine samples with a recovery of 98%-105%. A possible mechanism for this sensitized CL reaction is discussed by comparing the CL spectra with the fluorescence emission spectra. The proposed method represents a wide linear range, high sensitivity and accuracy, and can be used for the routine determination of ENX in pharmaceutical preparations and biological fluids.
首次开发了一种基于流动注射进样的新型三价镝(Dy(3+))敏化化学发光法,用于测定依诺沙星(ENX),该方法基于Dy(3+)-铈(Ce(IV))-S₂O₃²⁻-ENX体系以及Dy(3+)-高锰酸根(MnO₄⁻)-S₂O₃²⁻-ENX体系反应产生的化学发光(CL)。研究并优化了化学发光发射的分析条件。依诺沙星的化学发光强度与其浓度之间具有良好的线性关系,相关系数为0.9984 - 0.9994。对于Dy(3+)-ENX-S₂O₃²⁻-Ce(IV)-H₂SO₄体系,检测限(LOD,3σ)为0.20 ng/mL;对于Dy(3+)-ENX-S₂O₃²⁻-MnO₄⁻-HNO₃体系,检测限为0.22 ng/mL。对60 ng/mL依诺沙星进行11次测定,相对标准偏差(RSD,n = 11)为1.8%。该方法应用于注射液、血清和尿液样品中依诺沙星的分析,回收率为98% - 105%。通过比较化学发光光谱和荧光发射光谱,讨论了这种敏化化学发光反应的可能机制。该方法具有宽线性范围、高灵敏度和准确性,可用于药物制剂和生物流体中依诺沙星的常规测定。