Skip to Content
Merck
  • Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis.

Journal of chromatography. A (2014-06-19)
Rita Celano, Anna Lisa Piccinelli, Luca Campone, Luca Rastrelli
ABSTRACT

Pharmaceutical and personal care products (PPCPs) are one of the most important classes of emerging contaminants. The potential of ecological and environmental impacts associated with PPCPs are of particular concern because they continually penetrate the aquatic environment. This work describes a novel ultra-preconcentration technique for the rapid and highly sensitive analysis of selected PPCPs in environmental water matrices at ppt levels. Selected PPCPs were rapidly extracted and concentrated from large volumes of aqueous solutions (500 and 250mL) by solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and then analyzed using UHPLC-MS/MS. Experimental parameters were carefully investigated and optimized to achieve the best SPE-DLLME efficiency and higher enrichment factors. The best results were obtained using the ternary mixture acetonitrile/methanol/dichloromethane 3:3:4, v/v/v, both as SPE eluent and DLLME extractant/dispersive mixture. DLLME aqueous solution (5% NaCl, 10mgL(-1) TBAB) was also modified to improve the extraction efficiency of more hydrophilic PPCPs. Under the optimal conditions, an exhaustive extraction for most of the investigated analytes (recoveries >70%), with a precision (RSD <10%) and very high enrichment factors were attained for different aqueous matrices (drinking, sea, river and wastewater). Method detection and quantification limits were at very low ppt levels and below 1 and 3ngL(-1), respectively, for 15 of selected PPCPs. The proposed analytical procedure offers numerous advantages such as the simplicity of operation, rapidity, a high enrichment factor and sensitivity. So it is suitable for monitoring and studies of occurrence of PPCPs in different environmental compartments.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Dichloromethane, suitable for HPLC, ≥99.9%, contains 40-150 ppm amylene as stabilizer
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, JIS special grade, ≥99.0%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, SAJ first grade, ≥99.0%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Butyl 4-hydroxybenzoate, SAJ first grade, ≥99.0%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, JIS 300, for residue analysis
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, JIS 5000, for residue analysis
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, HPLC grade
SKU
Pack Size
Availability
Price
Quantity
Supelco
Dichloromethane solution, certified reference material, 5000 μg/mL in methanol
SKU
Pack Size
Availability
Price
Quantity
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, ≥99.5%, ACS reagent
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
2-Ethylhexyl salicylate, ≥99%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Butyl 4-hydroxybenzoate, ≥99%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Methanol, suitable for HPLC
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Methanol, SAJ special grade
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, for residue analysis, JIS 5000
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Ethyl 4-hydroxybenzoate, SAJ first grade, ≥99.0%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 300
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, for chromatography
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, JIS special grade, ≥99.5%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Ammonium acetate solution, 50 % (w/v), for copper determination
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Acetonitrile, ≥99.8%, suitable for HPLC
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
SKU
Pack Size
Availability
Price
Quantity
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
SKU
Pack Size
Availability
Price
Quantity