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An Ultraperformance Liquid Chromatography Tandem-Mass Spectrometry Method for Determination of Multiclass Pharmaceuticals in Water Sample by Dispersive Liquid-Liquid Microextraction Combined with Ultrasound Assisted Reverse Extraction from Solidified Floating Organic Droplets.

ABSTRACT: A novel, simple, and reliable ultraperformance liquid chromatography tandem-mass spectrometry (UPLC-MS/MS ) assay based on dispersive liquid-liquid microextraction followed by ultrasound-assisted reverse extraction from solidified floating organic droplets was established for determination of multiclass pharmaceuticals in the water sample. Six commonly used drugs of various therapeutic classes: ibuprofen, ketorolac, lamotrigine, propranolol, pantoprazole, and losartan were extracted from water samples by using 50 μL 1-undecanol as extracting solvent and 400 μL acetonitrile as dispersive solvent. After collecting the floating organic droplets by cold centrifugation, an ultrasound-assisted back extraction procedure was performed to make the sample compatible for UPLC-MS/MS analysis. Acquity BEH C₁₈ column (2.1 × 100; 1.7 μm) was used for separation of target analytes that were eluted by a gradient mobile phase composition of 15 mM ammonium acetate and acetonitrile at a flow rate of 0.25 mL/min. The sample ionization was performed by using electrospray ionization in positive mode, and multiple reaction monitoring was used for quantification of target analytes. After optimizing the assay conditions, all calibration curves were found to be linear with limit of detection and limit of quantification were ranged in between 0.06-0.15 and 0.16-0.41 ng/mL, respectively. The enrichment factor was found to be 172-192-fold and the relative recovery was ranged between 93.1 and 109.4% between target analytes. These satisfactory results confirmed that the proposed method is specific and reliable for application of trace analysis of target analytes in waste water samples.

SUBMITTER: Iqbal M

PROVIDER: S-EPMC7992067 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:DNA adducts are a measure of internal exposure to genotoxicants and an important biomarker for human risk assessment. However, the employment of DNA adducts as biomarkers in human studies is often restricted because fresh-frozen tissues are not available. In contrast, formalin-fixed paraffin-embedded (FFPE) tissues with clinical diagnosis are readily accessible. Recently, our laboratory reported that DNA adducts of aristolochic acid, a carcinogenic component of Aristolochia herbs used in traditional Chinese medicines worldwide, can be recovered quantitatively from FFPE tissues. In this study, we have evaluated the efficacy of our method for retrieval of DNA adducts from archived tissue by measuring DNA adducts derived from four other classes of human carcinogens: polycyclic aromatic hydrocarbons (PAHs), aromatic amines, heterocyclic aromatic amines (HAAs), and N-nitroso compounds (NOCs). Deoxyguanosine (dG) adducts of the PAH benzo[a]pyrene (B[a]P), 10-(deoxyguanosin-N(2)-yl)-7,8,9-trihydroxy-7,8,9,10-tetrahydrobenzo[a]pyrene (dG-N(2)-B[a]PDE); the aromatic amine 4-aminobiphenyl (4-ABP), N-(deoxyguanosin-8-yl)-4-aminobiphenyl (dG-C8-4-ABP); the HAA 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP), N-(deoxyguanosin-8-yl)-PhIP (dG-C8-PhIP); and the dG adducts of the NOC 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), O(6)-methyl-dG (O(6)-Me-dG) and O(6)-pyridyloxobutyl-dG (O(6)-POB-dG), formed in liver, lung, bladder, pancreas, or colon were recovered in comparable yields from fresh-frozen and FFPE preserved tissues of rodents treated with the procarcinogens. Quantification was achieved by ultraperformance liquid chromatography coupled with electrospray ionization ion-trap multistage mass spectrometry (UPLC/ESI-IT-MS(3)). These advancements in the technology of DNA adduct retrieval from FFPE tissue clear the way for use of archived pathology samples in molecular epidemiology studies designed to assess the causal role of exposure to hazardous chemicals with cancer risk.

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An Ultraperformance Liquid Chromatography Tandem-Mass Spectrometry Method for Determination of Multiclass Pharmaceuticals in Water Sample by Dispersive Liquid-Liquid Microextraction Combined with Ultrasound Assisted Reverse Extraction from Solidified Floating Organic Droplets.

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