This document describes a method for the analysis of chloropropanols in hydrolyzed vegetable protein using selected ion storage. The method is based on the capillary GC of a heptafluorobutyrate derivative with electron capture detection (ECD) at an overall limit of detection of about 1.5 mg/kg, depending on the sample type (dry weight basis).
This document details an analytical method for detecting chloropropanols, specifically 3-monochloropropandiol (3-MCPD), in Hydrolysed Vegetable Protein (HVP). The method utilizes Selected Ion Storage (SIS) mode on a GC/MS system to overcome matrix interference and improve detection limits compared to traditional Electron Capture Detection (ECD).
The note provides the full experimental procedure, including sample preparation involving extraction with hexane/ether and derivatization using heptafluorobutyrylimidazole. It also lists specific instrument conditions for the gas chromatograph and mass spectrometer required to achieve a detection limit of approximately 0.01 mg/kg.
| Detection Limit | 0.01 mg/kg |
|---|---|
| Column Type | BPX5 25M X 0.2mm X 0.25um |
| Mass Range | 70-300u |
| Internal Standard | p-dichlorobenzene |
The limit of detection is about 0.01 mg/kg based on a spike of 0.05 mg/kg.
Quantitation is performed using p-dichlorobenzene as the internal standard.
Selected Ion Storage provides a 150-fold increase in detection sensitivity over existing procedures.