Automated polyvinylidene difluoride hollow fiber liquid-phase microextraction of flunitrazepam in plasma and urine samples for gas chromatography/tandem mass spectrometry.
A new polyvinylidene difluoride (PVDF) hollow fiber (200 microm wall thickness, 1.2mm internal diameter, 0.2 microm pore size) was compared with two other polypropylene (PP) hollow fibers (200, 300 microm wall thickness, 1.2mm internal diameter, 0.2 microm pore size) in the automated hollow fiber liquid-phase microextraction (HF-LPME) of flunitrazepam (FLNZ) in biological samples. With higher porosity and better solvent compatibility, the PVDF hollow fiber showed advantages with faster extraction efficiency and operational accuracy. Parameters of the CTC autosampler program for HF-LPME in plasma and urine samples were carefully investigated to ensure accuracy and reproducibility. Several parameters influencing the efficiency of HF-LPME of FLNZ in plasma and urine samples were optimized, including type of porous hollow fiber, organic solvent, agitation rate, extraction time, salt concentration, organic modifier, and pH. Under optimal conditions, extraction recoveries of FLNZ in plasma and urine samples were 6.5% and 83.5%, respectively, corresponding to the enrichment factor of 13 in plasma matrix and 167 in urine matrix. Excellent sample clean-up was observed and good linearities (r(2)=0.9979 for plasma sample and 0.9995 for urine sample) were obtained in the range of 0.1-1000 ng/mL (plasma sample) and 0.01-1000 ng/mL (urine sample). The limits of detection (S/N=3) were 0.025 ng/mL in plasma matrix and 0.001 ng/mL in urine matrix by gas chromatography/mass spectrometry/mass spectrometry.
Cui
Shufen
S
Department of Biological Applied Engineering, Shenzhen Polytechnic, Shenzhen, China. shufencui@163.com
Tan
Shuo
S
Ouyang
Gangfeng
G
Pawliszyn
Janusz
J
D001331:Automation; D005591:Chemical Fractionation / Q000379:methods*; D005445:Flunitrazepam / Q000097:blood* / Q000652:urine*; D008401:Gas Chromatography-Mass Spectrometry; D006863:Hydrogen-Ion Concentration; D008855:Microscopy, Electron, Scanning; D011145:Polyvinyls / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012965:Sodium Chloride / Q000737:chemistry; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry; D013997:Time Factors; D005465:Fluorocarbon Polymers
D005445:Flunitrazepam; D011145:Polyvinyls; D012965:Sodium Chloride; D012997:Solvents; C024865:polyvinylidene fluoride; D005465:Fluorocarbon Polymers