Development of analytical method for detection of some pharmaceuticals in surface water

Fouad Fadhil Al-Qaim, Md. Pauzi Abdullah, Mohamed Rozali Othman, Jalifah Latip, Wan Mohamed Afiq

Research output: Contribution to journalArticle

16 Citations (Scopus)

Abstract

Purpose: To develop and validate a simple method using solid - phase extraction along with liquid chromatography-time of flight mass spectrometry for the analysis of pharmaceuticals in surface water of Tangkas River, Malaysia. Methods: Liquid chromatography (LC) was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system equipped with a vacuum degasser, a quaternary pump, an autosampler and UV-Vis diod array detector. Chromatography was performed on a Thermo Scientific C18 (250 mm x 2.1 mm, i.d.: 5μm) column. The injection volume was 20 μL. All compounds (hydrochlorothiazide, gliclazide, diclofenac-Na and mefenamic acid) were analysed in negative ion (NI) mode and eluted off the column with a mobile phase consisting of (A) 0.1% formic acid (FA) in deionised water (DIW) and (B) 40% acetonitrile (ACN) in methanol (MeOH) at 0.3 ml/min. Mass spectrometry was performed on a time of flight (TOF) instrument. Results: The linearity range, 5 - 500 ng/mL, provided a determination coefficient (R2) > 0.99 for all compounds. The limit of detection (LOD) ranged from 65 - 136 ng/L while recovery ranged from 45 - 111.2 % in the river water. Two pharmaceutical compounds were detected in the surface water samples: diclofenac sodium and mefenamic acid at concentrations of 340 and 545 ng/L, respectively. Conclusion: The developed method is linear in the range 5 - 500 ng/mL, and precise and acceptable recoveries were obtained. In addition, this method is suitable to identify and quantify trace concentrations of diclofenac sodium and mefenamic acid in surface water.

Original languageEnglish
Pages (from-to)609-616
Number of pages8
JournalTropical Journal of Pharmaceutical Research
Volume12
Issue number4
DOIs
Publication statusPublished - 2013

Fingerprint

Mefenamic Acid
Diclofenac
Water
Liquid Chromatography
formic acid
Pharmaceutical Preparations
Rivers
Mass Spectrometry
Gliclazide
Hydrochlorothiazide
Malaysia
Solid Phase Extraction
Vacuum
Methanol
Limit of Detection
Chromatography
Ions
Injections

Keywords

  • Collision energy
  • Diclofenac
  • Electrospray Ionization
  • Mass spectrometry
  • Mefenamic acid
  • Solid phase extraction (SPE)
  • Tangkas river

ASJC Scopus subject areas

  • Pharmaceutical Science
  • Pharmacology (medical)

Cite this

Development of analytical method for detection of some pharmaceuticals in surface water. / Al-Qaim, Fouad Fadhil; Abdullah, Md. Pauzi; Othman, Mohamed Rozali; Latip, Jalifah; Afiq, Wan Mohamed.

In: Tropical Journal of Pharmaceutical Research, Vol. 12, No. 4, 2013, p. 609-616.

Research output: Contribution to journalArticle

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abstract = "Purpose: To develop and validate a simple method using solid - phase extraction along with liquid chromatography-time of flight mass spectrometry for the analysis of pharmaceuticals in surface water of Tangkas River, Malaysia. Methods: Liquid chromatography (LC) was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system equipped with a vacuum degasser, a quaternary pump, an autosampler and UV-Vis diod array detector. Chromatography was performed on a Thermo Scientific C18 (250 mm x 2.1 mm, i.d.: 5μm) column. The injection volume was 20 μL. All compounds (hydrochlorothiazide, gliclazide, diclofenac-Na and mefenamic acid) were analysed in negative ion (NI) mode and eluted off the column with a mobile phase consisting of (A) 0.1{\%} formic acid (FA) in deionised water (DIW) and (B) 40{\%} acetonitrile (ACN) in methanol (MeOH) at 0.3 ml/min. Mass spectrometry was performed on a time of flight (TOF) instrument. Results: The linearity range, 5 - 500 ng/mL, provided a determination coefficient (R2) > 0.99 for all compounds. The limit of detection (LOD) ranged from 65 - 136 ng/L while recovery ranged from 45 - 111.2 {\%} in the river water. Two pharmaceutical compounds were detected in the surface water samples: diclofenac sodium and mefenamic acid at concentrations of 340 and 545 ng/L, respectively. Conclusion: The developed method is linear in the range 5 - 500 ng/mL, and precise and acceptable recoveries were obtained. In addition, this method is suitable to identify and quantify trace concentrations of diclofenac sodium and mefenamic acid in surface water.",
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AU - Othman, Mohamed Rozali

AU - Latip, Jalifah

AU - Afiq, Wan Mohamed

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AB - Purpose: To develop and validate a simple method using solid - phase extraction along with liquid chromatography-time of flight mass spectrometry for the analysis of pharmaceuticals in surface water of Tangkas River, Malaysia. Methods: Liquid chromatography (LC) was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system equipped with a vacuum degasser, a quaternary pump, an autosampler and UV-Vis diod array detector. Chromatography was performed on a Thermo Scientific C18 (250 mm x 2.1 mm, i.d.: 5μm) column. The injection volume was 20 μL. All compounds (hydrochlorothiazide, gliclazide, diclofenac-Na and mefenamic acid) were analysed in negative ion (NI) mode and eluted off the column with a mobile phase consisting of (A) 0.1% formic acid (FA) in deionised water (DIW) and (B) 40% acetonitrile (ACN) in methanol (MeOH) at 0.3 ml/min. Mass spectrometry was performed on a time of flight (TOF) instrument. Results: The linearity range, 5 - 500 ng/mL, provided a determination coefficient (R2) > 0.99 for all compounds. The limit of detection (LOD) ranged from 65 - 136 ng/L while recovery ranged from 45 - 111.2 % in the river water. Two pharmaceutical compounds were detected in the surface water samples: diclofenac sodium and mefenamic acid at concentrations of 340 and 545 ng/L, respectively. Conclusion: The developed method is linear in the range 5 - 500 ng/mL, and precise and acceptable recoveries were obtained. In addition, this method is suitable to identify and quantify trace concentrations of diclofenac sodium and mefenamic acid in surface water.

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KW - Solid phase extraction (SPE)

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