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  • Simultaneous determination of polar pharmaceuticals and personal care products in biological organs and tissues.

Simultaneous determination of polar pharmaceuticals and personal care products in biological organs and tissues.

Journal of chromatography. A (2014-06-25)
Rumi Tanoue, Kei Nomiyama, Haruna Nakamura, Terutake Hayashi, Joon-Woo Kim, Tomohiko Isobe, Ryota Shinohara, Shinsuke Tanabe
ABSTRACT

In the present study, a sensitive and accurate isotope dilution method was developed for the simultaneous determination of 17 polar pharmaceutical and personal care product (PPCP) residues (logKow=1.40-5.74), including 14 pharmaceuticals and 3 personal care products, in biological organs and tissues. The proposed method involved enzymatic hydrolysis, followed by sequential clean-up using silica gel chromatography and gel permeation chromatography, and analysis via ultra-high-performance liquid chromatography with tandem mass spectrometry. This method yielded acceptable absolute recoveries (48-88%) and internal standard-corrected recoveries (90-130%) for 17 PPCPs. Method detection limits were between 0.0092 and 3.2ngg(-1) wet weight, and the limits of quantification were between 0.020 and 8.7ngg(-1) wet weight. The method can be used to readily detect the target compounds at trace levels while minimizing the required sample volume. The developed method was applied to the determination of 17 PPCPs in the liver and kidney of 17 birds collected from Japan and also in the plasma, liver, and brain of 7 cyprinoid fish from an effluent-dominated stream in Japan. Triclosan was detected in 5 of 11 fish-eating birds but not in non-fish-eating birds, suggesting the contamination of prey fish by the chemical. Non-steroidal anti-inflammatory drugs, antibacterial agents, and psychotropic agents were frequently detected in the fish tissues. In addition, 7 of the target compounds were found in fish brain. The median brain/plasma ratios of the psychotropic agents ranged from 1.6 (carbamazepine) to 12 (diphenhydramine), indicating high transportability to fish brain.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Carbamazepine, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Indomethacin, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Indomethacin, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetone, natural, ≥97%
USP
Acetone, United States Pharmacopeia (USP) Reference Standard
Carbamazepine, European Pharmacopoeia (EP) Reference Standard
Bezafibrate, European Pharmacopoeia (EP) Reference Standard
Supelco
Mefenamic acid, analytical standard
USP
Indomethacin, United States Pharmacopeia (USP) Reference Standard
USP
Ibuprofen, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Carbamazepine, meets USP testing specifications
Sigma-Aldrich
Carbamazepine, powder
Sigma-Aldrich
Ammonium acetate, Molecular Biology, ≥98%
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonium acetate, BioUltra, ≥99.0%
Sigma-Aldrich
Ammonium acetate solution, BioUltra, ~5 M in H2O
Supelco
Acetone, analytical standard
Sigma-Aldrich
Ibuprofen, meets USP testing specifications
Sigma-Aldrich
Indomethacin, 98.5-100.5% (in accordance with EP)
Sigma-Aldrich
Bezafibrate, ≥98%, solid