Drugs of abuse and tranquilizers in Dutch surface waters, drinking ...

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RIVM Report 703719064Appendix B HPLC-MS/MS at RIVMRIVM developed an analytical method based on the method that is described byHuerta-Fontela et al. (2007). This method is summarised in Figure B.1.A short explanation of the performed procedureThe compounds were extracted from the water samples by means of solid-phaseextraction and analysed with HPLC-MS/MS (Quattro Ultima triple quadrupolemass spectrometer, Waters).The most abundant product ion of each compound was used for quantificationand the second one for confirmation (Table B.1). The sample was consideredpositive when this ion ratio fell within the tolerance range described in EUdirective 2002/657/EC.50 mL 100 mL water water sample sample * *+ internal standard(~20 ng/L)SPEOasis Oasis MCX, HLB, 150mg 200 mg cartridgesCONDITIONING :6 mL MeOH9 mL Milli - Q waterELUTION :6mL0.1%formicacidinMeOHEvaporation at 35°C under NitrogenExtractReconstitution, 400 µL 5% MeOHwith 0.1% formic acid(aq)25 µLUHPLC -MS/MS* Sample five - times diluted in the case of influent wastewaterFigure B.1 Diagram of the RIVM procedurePage 57 of 90
RIVM Report 703719064Table B.1. HPLC-MS/MS parameters established for the SRM acquisition mode(quantification and confirmation transitions). For isotope labelled internalstandards, only one transition was acquiredCompounds Precursor ion CV a CE b Product ion c(m/z) [M + H] + (V) (eV) (m/z)Amphetamine 136.4 15 15 91.410 119.2Methamphetamine 150.6 15 20 91.410 119.2MDA 180.4 20 10 163.425 133.1MDMA 194.5 40 10 163.325 105.2MDEA 208.5 15 15 163.325 105.2Ketamine 238.5 15 25 125.315 220.3Benzoylecgonine 290.6 10 20 168.435 105.2Cocaine 304.3 35 20 182.435 105.2Phencyclidine 244.6 25 15 86.215 159.4LSD 324.8 25 20 223.430 208.2Fentanyl 337.4 35 40 105.225 188.4Flunitrazepam 314.6 10 25 268.435 239.2Amphetamine-d 8 144.4 15 10 127.2Methamphetamine-d 9 159.6 15 10 125.2MDA-d 5 185.4 20 10 168.4MDMA-d 5 199.5 40 10 165.3MDEA-d 5 213.5 15 15 163.3Ketamine-d 4 242.5 15 25 129.3Benzoylecgonine-d 3 293.6 10 20 171.4Cocaine-d 3 307.3 35 20 185.4Phencyclidine-d 5 249.6 25 15 86.2LSD-d 3 327.8 25 20 226.4Fentanyl-d 5 342.4 35 40 105.2Flunitrazepam-d 7 321.6 10 25 275.4a CV, cone voltage; b CE, collision energy; c Top, product ion used for quantification (Q);Below, the product ion used for confirmation (q).Page 58 of 90
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Page 33 and 34: RIVM Report 703719064Ouddorp70ng/l6
Page 35 and 36: RIVM Report 703719064Bankfiltrate70
Page 37 and 38: RIVM Report 7037190643.3 Estimated
Page 39 and 40: RIVM Report 703719064further resear
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Page 43 and 44: RIVM Report 703719064An illustrativ
Page 45 and 46: RIVM Report 703719064concentration
Page 47 and 48: RIVM Report 703719064Barbiturates a
Page 49 and 50: RIVM Report 703719064Further resear
Page 51 and 52: RIVM Report 703719064Huerta-Fontela
Page 55 and 56: RIVM Report 703719064This LOQ estim
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Page 66 and 67: RIVM Report 703719064Appendix C HPL
Page 68 and 69: RIVM Report 703719064Table C.3 pres
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Page 74 and 75: RIVM Report 703719064LEGEND - below
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Page 78 and 79: RIVM Report 703719064Chemical class
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Page 86 and 87: RIVM Report 703719064carcinogenicit
Page 88 and 89: RIVM Report 703719064provisional dr
Page 90 and 91: RIVM Report 703719064ReferencesAmio
Page 92: N.G.F.M. van der Aa | E. Dijkman |
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