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Multi-residue analytical methodology-based liquid chromatography-time-of-flight-mass spectrometry for the analysis of pharmaceutical residues in surface water and effluents from sewage treatment plants and hospitals.

Journal of chromatography. A (2014-04-29)
Fouad F Al-Qaim, M P Abdullah, Mohamed R Othman, Jalifah Latip, Zuriati Zakaria
ABSTRACT

An analytical method that facilitated the analysis of 11 pharmaceuticals residue (caffeine, prazosin, enalapril, carbamazepine, nifedipine, levonorgestrel, simvastatin, hydrochlorothiazide, gliclazide, diclofenac-Na, and mefenamic acid) with a single pre-treatment protocol was developed. The proposed method included an isolation and concentration procedure using solid phase extraction (Oasis HLB), a separation step using high-performance liquid chromatography, and a detection procedure that applies time-of-flight mass spectrometry. The method was validated for drinking water (DW), surface water (SW), sewage treatment plant (STP) influent and effluent, and hospital (HSP) influent and effluent. The limits of quantification were as low as 0.4, 1.6, 5, 3, 2.2 and 11 ng/L in DW, SW, HSP influent and effluent, STP effluent, and STP influent, respectively. On average, good recoveries higher than 75% were obtained for most of the target analytes in all matrices. Matrix effect was evaluated for all samples matrices. The proposed method successfully determined and quantified the target compounds in raw and treated wastewater of four STPs and three hospitals in Malaysia, as well as in two SW sites. The results showed that a number of the studied compounds pose moderate to high persistency in sewage treatment effluents as well as in the recipient rivers, namely; caffeine, simvastatin, and hydrochlorothiazide. Ten out of 11 compounds were detected and quantified in 13 sampling points. Caffeine was detected with the highest level, with concentrations reaching up to 9099 ng/L in STP influent.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Nifedipine, ≥98% (HPLC), powder
Supelco
Melting point standard 235-237°C, analytical standard
Supelco
Carbamazepine, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Nifedipine, United States Pharmacopeia (USP) Reference Standard
Nifedipine, European Pharmacopoeia (EP) Reference Standard
USP
Carbamazepine, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Mefenamic acid
Supelco
D(−)-Norgestrel, analytical standard
Sigma-Aldrich
Carbamazepine, powder
Sigma-Aldrich
Carbamazepine, meets USP testing specifications
Mefenamic acid, European Pharmacopoeia (EP) Reference Standard
Caffeine for system suitability, European Pharmacopoeia (EP) Reference Standard
Supelco
Mefenamic acid, analytical standard
Carbamazepine, European Pharmacopoeia (EP) Reference Standard
Levonorgestrel for system suitability 2, European Pharmacopoeia (EP) Reference Standard
Supelco
Carbamazepine, analytical standard
Supelco
Nifedipine, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Caffeine, Sigma Reference Standard, vial of 250 mg
Sigma-Aldrich
Caffeine, meets USP testing specifications, anhydrous
Sigma-Aldrich
Hydrochlorothiazide, meets USP testing specifications
Sigma-Aldrich
Caffeine, powder, ReagentPlus®
Sigma-Aldrich
Hydrochlorothiazide, crystalline
Sigma-Aldrich
Caffeine, BioXtra
Sigma-Aldrich
Gliclazide, powder, ≥98%
Supelco
Hydrochlorothiazide, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Caffeine Melting Point Standard, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Caffeine, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Caffeine, anhydrous, 99%, FCC, FG
Supelco
Mettler-Toledo Calibration substance ME 18872, Caffeine, analytical standard, for the calibration of the thermosystem 900, traceable to primary standards (LGC)
Sigma-Aldrich
Caffeine, anhydrous, tested according to Ph. Eur.