Evaluation of selected pharmaceuticals and personal care products in water matrix using ion trap mass spectrometry: A simple weighted calibration curve approach

Gopal, Chikmagalur and Bhat, Krishnamurthy and Reddy, Praveen Kumar Y and shailesh, . and Kumar, Virendra and Basu, Hirakendu and Joshua, DerrickIan and Singhal, Rakesh Kumar and Balakrishna, K (2020) Evaluation of selected pharmaceuticals and personal care products in water matrix using ion trap mass spectrometry: A simple weighted calibration curve approach. Journal of Pharmaceutical and Biomedical Analysis, 113214. ISSN 2230 – 7885

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Abstract

A novel analytical method is presented for 12 target pharmaceutical and personal care products (PPCPs), belonging to different classes like antibiotics, non-steroid anti-inflammatory drugs, parabens, UV-filters, plasticizer, and antibacterials. The method development comprises of solid-phase extraction (SPE) with lipophilic–hydrophilic material balanced Oasis HLB cartridge, followed by reverse-phase liquid chromatography interfaced to linear ion trap tandem mass spectrometry (LC–MS/MS) with electrospray ionization. Chromatographic separation was achieved with a gradient elution of 25 min run time using 5 mM ammonium acetate buffer with pH adjustment using acetic acid. In addition, cost effective organic solvent with buffer used together as the mobile phase with Chromatopak C18 column (150 mm × 4 mm, 5-m,) in negative ionization mode. Recoveries ranged from 61.74 % to 119.89 % for most of the compounds. Matrix-matched calibration curves were used for counterbalancing the matrix effects for all the analytes, and ibuprofen D3 internal standard was used for assessing the effectiveness of extraction technique and monitoring the recovery of sample analysis. Simple empirical weighted linear regression curve technique was adopted practically for each analysis in enhancing the analyte accuracy at lower quantification level. The 1/x2 model was selected as the best suitable model for quantification of analytes, which can be evaluated by deviation from back-calculated concentration in terms of percentage relative error (%RE). Weighted calibration curves with regression value for most of the compounds were ≥ 0.98, except triclosan with a regression value ≥ 0.93. Precision showed as % relative standard deviation (%RSD) were always below 15.0 %. Accuracy-test was evaluated by the statistical one-sample t-test and no significant difference was observed between nominal and experimental value. The limit of quantification (LOQ) ranged from 3.0 ng/mL (BP1) to 1000 ng/mL (naproxen). Finally, the validated method was used for the first time to determine target analytes in surface water samples collected from Arkavathi river flowing across southern India’s Bengaluru city.

Item Type: Article
Uncontrolled Keywords: Arkavathi river Bengaluru Oasis HLB PPCPs Tandem-Mass spectrometer Weighting model
Subjects: Engineering > MIT Manipal > Civil Engineering
Depositing User: MIT Library
Date Deposited: 25 Jun 2020 06:41
Last Modified: 25 Jun 2020 06:41
URI: http://eprints.manipal.edu/id/eprint/155270

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