The Analysis Of DHA In The Plasma And Polychlorinated Biphenyls In The Water By Tandem Mass Spectrometry

In recent years, the LC-MS and GC-MS techniques have become routine analysis instruments, but as the sample matrixes are more and more complex, more and more kinds of materials to be detected, the chromatography-mass spectrometry system in many cases have been unable to meet the detection requirements. Due to its better anti-interference, higher sensitivity and the ability of quantitative analysis, the tandem mass spectrometry has become a hot spot in the development of mass spectrometry. It has a wide range of applications in drug metabolism, proteomics research, food safety, environmental monitoring and other fields. This paper analyzed DHA in the plasma and polychlorinated biphenyls in the water by tandem mass spectrometry.For the analysis of DHA, first of all,2-amino-2-methyl-1-propanol (AMP) was used as the heterocyclic derivative reagent for DHA in the plasma, and a gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis method was established. The reaction condition was optimized and used the internal standard curves method for the quantitation. In the range of0.07-10.00μg/mL, it had a good linear and r2=0.9991; the limit of quantitation was0.07μg/mL, and the limit of detection was0.02μg/mL; the average recoveries were96.00%-104.16%. And the group of20human plasma samples were analyzed, the concentration of DHA were1.532-2.524μg/g. Secondly, I used C18solid phase extraction (SPE) column to purify the plasma sample, and established a HPLC-MS/MS analysis method for DHA. Selecting reaction monitoring (SRM) pattern was used to detect DHA in this method, and external standard curves method was used for the quantitation. In the range of0.10-60.00μg/mL, the linear was good and r2=0.9990; the limit of quantitation was0.10μg/mL, and the limit of detection was0.04μg/mL; the average recoveries were94.79%-101.09%. And the group of20rat’s plasma samples were analyzed, the concentration of DHA were1.13-2.07μg/mL. The methods were both suitable for detecting DHA in the plasma.For the analysis of PCBs, this paper was using dispersive liquid-liquid microextraction (DLLME) method to extract the water, and established a gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis method which can simultaneously detect10kinds of PCBs. Then orthogonal experimental was adopted to study the five factors of DLLME. Through systematic study,in the range of2.5-1000.0ng/L,10kinds of PCBs all had good linears, and r2>0.9990; the limit of detections were from0.1ng/L to0.5ng/L, and the limit of quantitations were from0.4ng/L to2.5ng/L. At three spiked levels, the average recoveries were91.60%-108.03%,95.40%-109.08%and90.43%-105.52%respectively. Then I analyzed different sources of water with this method, only environmental water samples detected some PCBs, mineral water and tap water samples were not detected.