Combined solid‐phase extraction and gas chromatography–mass spectrometry used for determination of chloropropanols in water

Abstract

A sensitive and rapid derivatization method for the simultaneous determination of 1,3-dichloro-2-propanol (1,3-DCP) and 3-chloropropane-1,2-diol (3-MCPD) in water samples has been developed. The aim was to research the optimal conditions of the derivatization process for two selected reagents. A central composite design was used to determine the influence of derivatization time, derivatization temperature and reagent volume. A global desirability function was applied for multi-response optimization. The analysis was performed by gas chromatography-mass spectrometry. During the optimization of the extraction procedure, four different types of solid-phase extraction (SPE) columns were tested. It was demonstrated that the Oasis HLB cartridge produced the best recoveries of the target analytes. The pH value and the salinity were investigated using a Doehlert design. The best results for the SPE of both analytes were obtained with 1.5 g of NaCl and pH 6. The proposed method provides high sensitivity, good linearity (R(2)≥0.999) and repeatability (relative standard deviations % between 2.9 and 3.4%). Limits of detection and quantification were in the range of 1.4-11.2 ng/mL and 4.8-34.5 ng/mL, respectively. Recoveries obtained for water samples were ca. 100% for 1,3-DCP and 3-MCPD. The method has been successfully applied to the analysis of different samples including commercially bottled water, an influent and effluent sewage.

Optimization of ultrasonic‐assisted extraction of 3‐monochloropropane‐1,2‐diol (MCPD) and analysis of its esters from edible oils by gas chromatography–mass spectrometry

“…The results showed that 20% MTBE was optimal for the extraction of 3‐MCPD and its esters from the oil. These results were consistent with previous findings that concentrations of ethyl acetate and MTBE played an important role in the extraction of 3‐MCPD and its esters from oil and fat‐based matrices . It indicates that it is necessary to take into account the polarity of organic solvents involved in the dilution and transesterification of lipophilic 3‐MCPD esters and hydrophilic 3‐MCPD.…”

“…The results showed that 20% MTBE was optimal for the extraction of 3-MCPD and its esters from the oil. These results were consistent with previous findings that concentrations of ethyl acetate and MTBE played an important role in the extraction of 3-MCPD and its esters from oil and fat-based matrices [22,31,32]. It indicates that it is…”

3‐Chloropropane‐1,2‐diol (3‐MCPD) in Soy Sauce: A Review on the Formation, Reduction, and Detection of This Potential Carcinogen

“…The detection limit was 0.04 mg/kg. Gonzalez and others () combined solid‐phase extraction with GC‐MS to compare the efficiency of the derivatizing activities of BSTFA and HFBI. It was found that the LOD for BSTFA is 1.12 × 10 −2 mg/kg, which is low enough to quantify 3‐MCPD according to the EU.…”

Doehlert uniform shell designs and chromatography

“…An increased implementation of Doehlert uniform shell designs in GC-MS has been observed in the last decade for developing efficient sample treatment methods by monitoring different analytical functions such as recovery [49][50][51][52][53][54][55], analytical signal [56][57][58][59][60][61] and reaction yield [51,62]. Table 4 also shows that regardless of the potential benefits of uniform shell designs, they have not gained widespread popularity among researchers for optimizing systematically and simultaneously GC-MS instrumental variables.…”