环境水中有机污染物检测方案

This job shows a very rapid and effective method using all the most of the features of a QqLIT system to get very good sensitivity and identification capabilities. Using MRM transition to quantitate and MS/MS spectrum obtainedwith the Linear lon Trap for identification purposes is possible to work with a low resolution system and found unknown compounds from a pre-target list.CCANACMCA DETERMINATION OF EMERGING ORGANIC POLLUTANTS IN WASTEWATER BY“ON-LINE SPE”LC/QqLIT AND IDENTIFICATION BY MS/MS SPECTRUM N. Bellos， L. Bonettol， J.F. Rodriguez， F.A. Mocholi 1SAILab， Argenters， 5 Ed I bD. PTV.08290 Cerdanyola del Valles. Barcelona， Spain. fm@sailab.es ?TEKNIKER， Otaola 20·20600 Eibar· Gipuzkoa， Spain. INTRODUCTION INSTRUMENTATION Off-Line vs On-Line SPE Last years have been growing the interest in the quantitation ofpharmaceuticals and drugs， called Emerging Organic Contaminants(EOPs)， in drinking water or wastewater， in order to control the presenceof these compounds and to avoid future problems on the people. LC/MSis the appropriate technique because of the selectivity， good sensitivity，linearity and robustness. Problems had begun when confirmation oftarget compounds must to be done and identification of unknowncompounds is also needed. Mainly at very low concentrations， MRMratios are not so consistent for confirmation. Hybrid QTrap MS/MS(QqLIT) systems allow to do that confirmation issues. .“On-Line SPE”offer several features to improve the performance of themethod： less sample volume， less timework required， better recoveriesOnly1 ml sample is needed to achieve the detection limit required. EXPERIMENTAL Symbiosys Pico“On-Line SPE" automated system from Spark Holland coupled with 3200 QTrap'M LC/MS/MS system from ABSCIEX， have been the instrumentation used. “On-Line SPE" basics are depicted in the figure above.1 ml of sample was injected to the system. Previously cartridge (Hysphere 8um GP Resin， Spark Holland， Emmen， Holland).was conditioned and prepared for the extraction. Once the sample was applied， cartridge was washed and，then， mobile phase from the LC pump pass thru the cartridge to elute the analytes to the column. Steps， solvents and conditions are summarized in Table 1. Mobile phases were： Water， 2mM ammonia formiate， 0.1% formic acid (A)and acetonitrile (B). LC Gradient is shown in Table II. LC Column used was Luna C18(2)50mm， 2.1mm， 3um (Phenomenex， Torrance，CA，USA). Time(min) Solvent Flowrate(ml/min) A(%) (%) Conditioning Equilibration 00：01 00o 0.30 1000 80 Value Units Curtain Gas Nebulizer Voltage Water 01：00 0.30 1500 205500 500 pSY Turbo Temperature Water D.30 1000 9C psi System wash Turbo Gas 0.30 40 psi Collision Gas 2000 1000 High 0.30 80 80 20 Mass Spectrometer Turbo VTM source conditions are summarized in Table II. Acquisition has been made in MRM Mode and Identification of analytes has been made by QTrap via EPl and thru IDA criteria. Recognition of theacquired MS/MS spectra was done by comparison with commercial available "Forensic"Library from ABSCIEX. RESULTS AND DISCUSSION The method developed in this work include 114 compounds from different families shown In Table lV， together with the MRM conditions. This MRMs (one per compound) allow us to quantitate. Method has been validatedaccording EC 657/2002. CCa was found to be lower than 1 ug/l for all compounds arriving， individually， to 0.05 ug/. Linearity， precision and Accuracy wee inside accetable limits. Table IV.Analytes characteristics and MS/MS Conditions Caffeine Licit drug ( A n tib i ot i cs， anti-inflammatory，analge si cs， licit a n d il l ici t drug s， among o t h er ar e inc l uded in the l i st (Tabl e IV) . In the f i g ur e a bove ， s pectr a o f sev er a l c o mpound s of the m et ho d (the most common a p peared in t he sa m pl e s a r e s h o w n ( l e ft side)， co mpa r ed with t h e s p ec t ra c o m ing fro m the c omm er c ia l l i b ra ry (o n the r igh t ) ， show in g al l very g o od f it， over 80 %. ) CONCLUSIONS