Abstract
Antidiabetic drugs are among the most prescribed and consumed pharmaceuticals worldwide. Their occurrence in environment was little investigated due of lack of analytcial methods for their detection in waters. In this work has been developed a selective SPE-UHPLC/MS/MS method for isolation, identification and quantification of some antidiabetic compounds. The 3 selected analytes (glyburide, glimepiride and repaglinide) were separated on Eclipse C18 LC column at 300C using isocrat elution with mobile phase of acetonitrile: 0.04% acetic acid (60/40, v/v %). The optimal flow rate was 0.2 mL/min and the injected volum was 10 µL. The contaminants were detected in negative electropray ionization mode (ESI-) by Multiple Reaction Monitoring (MRM). Collision energy, fragmentor voltages were optimized to obtain high sensitivity. Optimization of SPE-LC-MS/MS parameters gave low quantification limit values between 0.27 and 11.1 ng/L. The organic pollutants were isolated from waste water samples on Strata C18 cartridges. The linear regressions were drawn in the interval of 1-100ng/L with good determination coefficients. Spike recovery rates were between 74.5 and 88.2% for waste water, with satisfactory precisions (RSD<15). the method was applied to analyze real influent and effluent of wastewater treatment plant (WWTP) samples. Keywords: antidiabetic contaminants, liquid chromatography-mass spectrometry, wastewater
Highlights
Antidiabetic drugs are among the most prescribed and consumed pharmaceuticals worldwide
Many of the pharmaceuticals do not degrade during wastewater treatment processes in municipal wastewater treatment plant (WWTP) and they are discharged into receiving surface waters, constituting major sources of contamination [914]
In order to establish the Multiple Reaction Monitoring (MRM) transitions, after obtaining the molecular ions of the compounds from the MS spectra, isolation and fragmentation were made in the collision cell to generate the product ions using the Product Ion Scan
Summary
Antidiabetic drugs are among the most prescribed and consumed pharmaceuticals worldwide. The aim of this work was to develop a new sensitive and selective SPE-LC/MS/MS method for the extraction and quantification of some antidiabetic contaminants in waste water samples and to evaluate their removal rate. This is the first national study about the antidiabetic’s occurrence in Romanian WWTPs. First the method was optimized for some working parameters of selective C18 solid phase extraction (SPE) and liquid-chromatograph equipped with QQQ (triple quadrupole) mass spectrometry (LC-MS/MS) in order to obtain low limits of quantification, high recovery rates and good precisions. The glass microfiber filters (1.6 μm) used to filtrate the samples were aqiured from Merck
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