Abstract

An ultrasensitive method for determining picomolar midecamycin (MID) by flow injection (FI) chemiluminescence (CL) was first described based on the inhibitory effect of MID on luminol–BSA reaction. It was found that the CL intensity decrements were linear with the logarithm of MID concentrations in the range of 1.0–5000 pmol · l–1with a detection limit as low as 0.3 pmol · l–1(3σ). The relative standard deviation of seven repetitive measurements for 10 pmol · l–1MID was 3.0%. At a flow rate of 2.0 ml · min–1, the whole analysis procedure including sampling and washing could be finished in 30 s, offering the sample efficiency of 120 h–1. This proposed method was successfully applied to determine MID in human serum samples with the recoveries from 96.0 to 110.0%. The CL mechanism of luminol–BSA–MID reaction was also given.

Highlights

  • Since flow injection (FI) analysis first described by Ruzicka and Hansen in 1975, it has revolutionized the performing way of analytical chemistry to a great extent [16]

  • It has been reported that the hyperchromic effect of BSA on luminol can accelerate the electrons transferring rate of excited 3-aminophthalate leading to the CL intensity of luminol remarkably enhanced, and this FI-CL system has been developed successfully to assay azithromycin in pharmaceutical preparations [21]

  • There has been no report on the determination of midecamycin (MID) by FI-CL using luminol–BSA system

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Summary

Introduction

Since flow injection (FI) analysis first described by Ruzicka and Hansen in 1975, it has revolutionized the performing way of analytical chemistry to a great extent [16]. High-performance liquid chromatography with evaporative light-scattering detection (HPLC-ELSD) is reported on determining MID [11]. In this present work, an ultrasensitive approach for determining MID by FI-CL was established for the first time on the basis of the inhibitory property of MID on luminol–BSA reaction. It was found that the CL intensity decrements were logarithm over MID concentrations, giving the calibration graph range of 1.0–5000 pmol · l−1 with the LOD of 0.3 pmol · l−1 (3σ) This proposed method was successfully applied to determine MID in human serum samples with the recoveries from 96.0 to 110.0%. The possible CL mechanism of luminol–BSA–MID reaction was discussed in detail

Reagents
Apparatus
Procedures
Treatment of spiked human serum samples
The relative CL intensity–time profile
Optimum conditions of luminol–BSA CL system
Analytical performance for the determination of MID
Interference studies
Possible CL mechanism of luminol–BSA–MID reaction
Determination of MID in spiked human serum samples
Conclusion
Methods

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