No abstract

A novel method of MSPD combined with DLLME for detecting 7 PBDEs in vegetables was developed by GC-MS/MS quantitation. Firstly, the freeze-dried vegetables were ground and blended with complex sorbents, and packed into a homemade column. PBDEs were eluted with only small amounts of organic solvent, collected and concentrated. Afterward, DLLME procedure was proceeded through addition of 5 mL of ultrapure water to the conical centrifuge tube for purification and pre-concentration. The optimal conditions in the MSPD and DLLME procedures were evaluated using single factor optimization. The results shown that sample weight was 0.2 g, a mixture of C18 and PSA was used as a composite sorbent with a dispersion ratio of 1:4, the elution solvent was a mixture of 8 mL n-hexane-dichloromethane (1:1,v/v) in MSPD process. After that, DLLME procedure was used 500 µl acetonitrile as dispersant and 35 µl carbon tetrachloride as extractant. The developed method showed a good linearity (R2 > 0.9992) between 1 and 1000 ng·g− 1 for all compounds, and matrix effects between − 3.3% and − 18.2%. Limits of detection (LODs) were between 0.08 and 1.00 ng·g− 1. Furthermore, the average recoveries of PBDEs were between 82.9% and 113.8% for all compounds, except for BDE 183 (between 58.5% and 82.5%) with the RSD of lower than 5.2%. This method proved to be saved-solvent, low-cost, eco-friendly, and efficient for the quantitative determination of PBDEs in actual vegetable samples under optimal conditions.

Herein, a novel pretreatment method for extraction of polybrominated diphenyl ethers (PBDEs) using matrix solid phase dispersion (MSPD) and depth purification using dispersive liquid–liquid micro-extraction (DLLME) from vegetables was designed.