Determination of the percentage of blood chlormezanone by GC/MS for clinical application on acute poisoning patients / 解放军医学杂志

ABSTRACT

Objective To develop a rapid and sensitive method for the determination of the percentage of blood chlormezanone by gas chromatograpy-mass spectrometry(GC/MS)for the clinical application on acute poisoning patients.Methods Chlormezanone in blood was extracted and separated with acetic ether.The acetic ether extractives from the blood were warmed with water at 80℃ and blown to dry with nitrogen gas.The dry extractives were then dissolved in 100?l of ethanol for GC/MS.To set up the linear equation for the determination of blood chlormezanone,draw the standard curve,calculate the extractive yield,detection limit and repeatability of chlormezanone.The GC was equipped with a 30m length,0.25mm I.D.,0.25?m film thickness HP-5MS(5% phenyl-methylpolysiloxane).Helium was used as the carrier gas at a constant flow rate of 1.0mL/min.The 1?l samples was injected GC/MS in split mode of 10∶1.The temperature program160℃ for 2min,10℃/min up to 280℃ and hold for 10min.The injector,MS quadrupole rods,ion source and transfer line were kept at 250℃,150℃,230℃ and 280℃,respectively.The EI electron impact energy was 70eV.Results The extractive yield with acetic ether for blood chlormezanone was 82.1%,RSD=6.6%,implying that and acetic ether is an ideal extraction solvent.The calibration curve was y=13 852x+140 588,r=0.998 2.The detection limit was 4?g/L(SCAN m/z 30-280)and 0.1?g/L(SIM m/z 98,152,154).The RSD of precision in one day was 2.6%.The RSD of the precision between days was 4.9%.Conclusions The extraction and analysis method is suitable to the diagnosis of the acute poisoning patient of chlormezanone.