Development of vial wall sorptive extraction and its application to determination of progesterone in human serum.
A novel sample preparation method, vial wall sorptive extraction (VWSE), which uses a vial whose internal wall is coated with polydimethylsiloxane (PDMS), was developed. The method was applied to the determination of progesterone in human serum sample. Human serum sample (0.5 mL) spiked with progesterone-13C2 was pipetted into the VWSE device and vortex mixing was performed for 30 min. Then, the serum sample was removed and the vial rinsed with purified water. Fifty microliter of methanol as liquid desorption (LD) solvent was pipetted into the VWSE device and vortex mixing was performed for 10 min. Then, the extract was analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The correlation coefficient (r) of the calibration curve over the concentration range of 0.5-200 ng mL(-1) was 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 and 0.5 ng mL(-1), respectively. The relative recoveries were 97.9% (RSD: 4.4%, n=6) and 102.8% (RSD: 1.1%, n=6) for progesterone spiked at 5 and 50 ng mL(-1), respectively. This simple, accurate, sensitive, and selective analytical method is applicable to the trace analysis of a minute amount of sample.
Kawaguchi
Migaku
M
Bio-Medical Standard Section, National Institute of Advanced Industrial Science and Technology (AIST), National Metrology Institute of Japan (NMIJ), 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan. m-kawaguchi@aist.go.jp
Fujii
Shin-ichiro
S
Itoh
Nobuyasu
N
Ito
Rie
R
Nakazawa
Hiroyuki
H
Takatsu
Akiko
A
D005591:Chemical Fractionation / Q000295:instrumentation* / Q000379:methods*; D002853:Chromatography, Liquid; D004129:Dimethylpolysiloxanes / Q000737:chemistry*; D006801:Humans; D011374:Progesterone / Q000097:blood*; D053719:Tandem Mass Spectrometry
D004129:Dimethylpolysiloxanes; D011374:Progesterone; C013830:baysilon