Trace‐level analysis of polychlorinated biphenyls, organochlorine pesticides and polycyclic aromatic hydrocarbons in human plasma or serum by dispersive liquid–liquid microextraction and gas chromatography–tandem mass spectrometry

Abstract

A method to determine 8 polychlorinated biphenyls (PCBs), 23 organochlorine pesticides (OCPs) and 16 polycyclic aromatic hydrocarbons (PAHs) was described using dispersive liquid-liquid microextraction (DLLME) of a small amount of plasma or serum sample and gas chromatography-tandem mass spectrometry (GC-MS/MS).The appropriate selection of the extraction solvent and dispersing solvent contributes to a high extraction yield and a clean extract. To verify the developed method, the interference, linearity of the calibration curve, detection limit, precision and accuracy were evaluated. The calibration curves were linear by 2-3 orders of magnitude with correlation coefficients above 0.997 in all cases. The LODs of PCBs, OCPs and PAHs were measured in the ranges of 0.0006-0.0029, 0.001-0.029 and 0.0002-0.012 ng/mL. The intraday precision achieved by this method was 2.19-10.3% (PCBs), 1.65-14.3% (OCPs) and 0.91-12.8% (PAHs), and the intraday accuracy 1.56-7.37% (PCBs), 2.34-19.6% (OCPs) and 1.49-15.7% (PAHs). The advantage of this method is that the analysis of PCBs, OCPs, and PAHs can be performed in a single chromatographic run, and the low detection limit enables monitoring of target substances in low exposure general public samples, and the analysis procedure is relatively simple and fast.

Review of scientific literature on available methods of assessing organochlorine pesticides in the environment

“…The carrier gas was helium (purity 99.99 %) with a flow rate of 1 Ml/min. RT: 15.27–22.29 min” [ 404 ] Plasma/serum 23 0.001–0.029 0.002–0.093 85.9–109 1.97–19.6 GC-MS/MS: “The oven temperature program was started at 70 °C, increased to 240 °C at 20 °C/min, and continuously increased to 310 °C at 8 °C/min and maintained at the final temperature for 11 min” [ 405 ] Plasma/serum 7) 0.02–0.07 4–40 GC-MS/MS: “The GC oven program was set to following values: 115 °C (2 min), 4 °C/min, 260 °C (1 min), 30 °C/min, 320 °C (2 min)” [ 406 ] serum 26 7 × 10 −5 -0.01344 30–124 HRMS/HRMS [ 407 ] Blood serum 11 74–120 <20 GC-MS/MS, UHPLC–MS/MS [ 101 ] Human tissue (liver, kidney, heart, spleen, lung, brain and abdominal fat) 20 1.0–16 85–109 <12 GTC-MS: “Splitless, the GC oven program started with an isothermal stage at 100 °C for 0.5 min, increasing at 10 °C/min ∼180 °C, and then at 2 °C/min ∼225 °C (2 min), to finally reach 265 °C at a rate of 20 °C/min, which was maintained for 1 min” [ 44 ] Human blood 8 0.004; 5 × 10 −5 ng a for detector Ave: 95 GC-ECD [ 408 ] ...…”

Application of instantaneous nebulization dispersive liquid‐phase microextraction combined with HPLC for the determination of chalcone and isoflavone in traditional Chinese medicines

“…In DLPME, the extractant and dispersant are injected into the sample solution at the same time, then the extractant is dispersed into tiny droplets for extraction, and finally it sinks to the bottom or floats on the liquid surface to achieve phase separation. Due to its simple operation, rapidity, and high enrichment factor (EF), it has been widely used in the extraction and enrichment of trace compounds in various complex matrices such as TCMs, food, environmental water, plasma, urine, and other samples [19][20][21][22][23].…”