| Polybrominated biphenyls(PBBs) has been widely used in the production of electronic electrical products of plastic and rubber parts as an excellent flame retardant effect of bromine flame retardants(BFRs). PBBs are persistent in natural conditions on the ground, for their persistence and hydrophobic, they are easy to combine with insoluble particles and enter the trophic chain. so as to have bioaccumulated in the blood, in breast milk, and in the fatty tissue of animals and humans. The mechanism of action underlying several of the toxicological effects of PBBs, among which are the induction of immunotoxicity, hepatotoxicity, and reproductive toxicity. The chemical properties of PBBs determine the applicability of the detection method, commonly used have chromatography(GC), high performance liquid chromatography(HPLC), mass spectrometry(MS) and electronic capture assay(ECD), etc.High performance liquid chromatography(HPLC) technology plays a very important role in the analysis of science, and has applied to many areas. Compared with gas chromatography(GC), especially for the poor thermal stability of compounds separation and analysis, HPLC has advantages of high sensitivity, analysis speed, wide range of applications and so on. However, for the analysis of complex sample matrices,HPLC often need to be combined with the sample preparation technique in order to improve the performance of the HPLC analysis.Ultrasound-assisted extraction technique is a simple, inexpensive and rapid method for pre-processing, and can effectively combine with HPLC for certain analytical purposes. Cloud point extraction technology developed rapidly in recent years, which can be applied to many areas of separation and analysis. It has advantages of low toxicity, sensitive, inexpensive and so on. This paper studies the determination of PBBs by HPLC combined with ultrasound-assisted extraction and cloud point extraction technology. Actually applied to the determination of PBBs residues in milk samples and environmental water samples. Details are as follows:Briefly introduces the research background of PBBs, reviewed the detection methods of PBBs and sample preparation techniques. Simply expounds the characteristics and development status of existing method.Established the ultrasound assisted extraction-high performance liquid chromatography method for measuring the PBBs in samples. Optimize the determination conditions of extraction and chromatography, extraction time 40 min,extraction temperature 40 ℃, ultrasonic time 5 min, centrifugal time 5 min, pH value5.5, gradient elution separation mode and mobile phase composition was 85% methanol15% water, etc. Under the optimal conditions, seven kinds of PBBs completely separated in 14 minutes. The RSD of retention time and peak area were 0.18%-0.33%and 4.24%-9.06% respectively. The LODs were 3.81-11.40 ng/m L. This method can be successfully applied to the analysis of PBBs residues in milk samples, and precision and recovery are generally good.Studied the analysis of PBBs in environmental water samples by cloud point extraction-high performance liquid chromatography. Discussed the main parameters affecting the performance of the method, as a result, the concentration of TX-114 was0.75%, additive concentration was 0.01 mol/L, extraction temperature was 50 ℃,extraction time was 20 min and so on. Under optimal conditions, seven kinds of PBBs completely separated within 14 minutes. The RSD of retention times and peak areas in the detection were 0.16%-0.34% and 1.04%-6.98%, the LODs were 3.01-67.42 ng/mL.This method can be successfully applied to the analysis of PBBs residues in environmental water samples, and the precision and recovery are better. |
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