Analysis of phthalates in wine using liquid chromatography tandem mass spectrometry combined with a hold-back column: Chromatographic strategy to avoid the influence of pre-existing phthalate contamination in a liquid chromatography system

• A simple, robust and reliable method was developed for measuring phthalates in wine.
• HPLC–MS/MS was practically used for wine phthalate analysis.
• No effect of HPLC phthalate contamination on analysis was confirmed.
• Extraction and enrichment were not required for sample preparation.

This paper describes the development and application of a novel method for the analysis of phthalates in wine using HPLC–MS/MS combined with a hold-back column. Phthalates are ubiquitous contaminants in the environment and can be widely found in laboratory materials and equipment. A HPLC system is no exception and can be the source of contamination affecting the accuracy and precision of analytical results. The new method successfully separates phthalates from the different sources, a wine sample and HPLC system by a simple technique using an additional HPLC column (a hold-back column) placed upstream of the injection valve. The hold-back column effectively retains the HPLC-derived contaminants during column equilibrium time and delays their elution times from an analytical column. Consequently, a phthalate from a wine sample can be baseline separated as it elutes sufficiently earlier than the same phthalate from the HPLC system. HPLC–MS/MS analysis combined with the hold-back column demonstrated virtually no influence of the HPLC contaminants on the quantification of phthalates present in wine. Together with a simple and rapid sample preparation and the use of labeled internal standards, the method was confirmed to be robust and reliable to determine concentrations of phthalates in wine. Quantification limits were within the range of 1.6–9.8 μg L−1 for dimethyl, diethyl, dibutyl, benzylbutyl, bis(2-ethylhexyl) and dioctyl phthalates, and 7.5–26.6 μg L−1 for multiple isomeric phthalates, di-iso-nonyl and di-iso-dodecyl phthalates.