MilliporeSigma
  • Home
  • Search Results
  • A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent.

A validated liquid chromatographic method for the determination of polycyclic aromatic hydrocarbons in honey after homogeneous liquid-liquid extraction using hydrophilic acetonitrile and sodium chloride as mass separating agent.

Journal of chromatography. A (2014-12-30)
Anastasia Koltsakidou, Constantinos K Zacharis, Konstantinos Fytianos
ABSTRACT

In the present report, a simple and cost-effective method for the determination of twelve US EPA priority polycyclic aromatic hydrocarbons (PAHs) in honey samples after salting-assisted liquid-liquid extraction and UHPLC with fluorescence detection is proposed. The sample treatment is based on the usage of hydrophilic acetonitrile as extraction solvent and its phase separation under high salinity conditions. Due to the high sugar content of the samples the phase separation is promoted effortlessly. Several parameters affecting the extraction efficiency and method sensitivity including the concentration of the honey samples, the type and volume of the extraction solvent, the type and quantity of the inorganic salt, extraction time and centrifugation time was systematically investigated. The method was validated in-house according to the Commission Decision 2002/657/EC guidelines. The limit of detection (LOD) of the method lay between 0.02 and 0.04ngmL(-1) (corresponding to 0.08 and 0.16ngg(-1)) which are close to the quality criteria established by European Regulation (EC) 836/2011 concerning the PAHs in foodstuffs. The mean analytical bias (expressed as relative recoveries) in all spiking levels was acceptable being in the range of 54-118% while the relative standard deviation (RSD) was lower than 19%. The proposed method has been satisfactorily applied for the analysis of the selected PAHs residues in various honey samples obtained from Greek region.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Magnesium sulfate solution, BioUltra, for molecular biology
Supelco
Ethanol standards 10% (v/v), 10 % (v/v) in H2O, analytical standard
Sigma-Aldrich
Isopropyl alcohol, ≥99.7%, FCC, FG
Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, 99.93%
Sigma-Aldrich
Acetone, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Ethanol Fixative 80% v/v, suitable for fixing solution (blood films)
Sigma-Aldrich
Magnesium sulfate solution, for molecular biology, 1.00 M±0.04 M
Supelco
Methanol, analytical standard
Supelco
Acetone, analytical standard
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 40.0% 2-propanol, 0.05% formic acid
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
USP
Dehydrated Alcohol, United States Pharmacopeia (USP) Reference Standard
Supelco
Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Dehydrated Alcohol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 0.1 % (v/v) formic acid, 5 % (v/v) water, suitable for HPLC
USP
Acetone, United States Pharmacopeia (USP) Reference Standard
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetone, Laboratory Reagent, ≥99.5%
Sigma-Aldrich
Acetone, ACS reagent, ≥99.5%
Sigma-Aldrich
Isopropyl alcohol, meets USP testing specifications
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free