title: Innovative microwave-assisted oximation and silylation procedures for metabolomic analysis of plasma samples using gas chromatography-mass spectrometry.
abstract: Analysis of plasma metabolomic samples by gas chromatography-mass spectrometry always requires comprehensive pretreatment including oximation and silylation. Although heating block (HB) is a commonly used method, it is time consuming. This study describes an extremely time-effective microwave-assisted (MA) oximation and silylation approach for metabolomic study of plasma samples. The Box-Behnken design was employed to optimize the MA conditions by means of oximation at 65 W for 100 s and then silylation through 180 s incubation with 230 W microwave irradiation. The results showed that microwave irradiation decreased the sample preparation time from approximately 180 min to 5 min without loss of information for the metabolites in plasma samples. Both the HB method and the developed MA method were applied in plasma metabolomic study of sulfur mustard intoxication. Partial least-squares discriminant analysis (PLS-DA) was used to globally understand the metabolic changes, and multi-criteria assessment was used to select the most significant and reliable variables as potential biomarkers. The data obtained by the MA method were in good correlation with the HB method. Compared with HB method, the newly developed MA oximation and silylation of plasma metabolome samples was more efficient and time-effective and may prove to be an attractive alternative for high-throughput sample preparation in plasma metabolomics.
authors: School of Pharmacy, Second Military Medical University, No. 325 Guohe Road, Shanghai 200433, China.
authors: Zhanying
authors: Z
authors: Hong
authors: Zebin
authors: Z
authors: Lin
authors: Yue
authors: Y
authors: Liu
authors: Guangguo
authors: G
authors: Tan
authors: Ziyang
authors: Z
authors: Lou
authors: Zhenyu
authors: Z
authors: Zhu
authors: Yifeng
authors: Y
authors: Chai
authors: Guorong
authors: G
authors: Fan
authors: Junping
authors: J
authors: Zhang
authors: Liming
authors: L
authors: Zhang
mesh_terms: D000596:Amino Acids / Q000097:blood; D000818:Animals; D001669:Biochemical Phenomena; D015415:Biomarkers / Q000032:analysis* / Q000097:blood / Q000378:metabolism; D001786:Blood Glucose / Q000378:metabolism; D016002:Discriminant Analysis; D004355:Drug Stability; D005690:Galactose / Q000097:blood; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D016018:Least-Squares Analysis; D055442:Metabolome / Q000187:drug effects; D055432:Metabolomics / Q000379:methods*; D008872:Microwaves; D009151:Mustard Gas / Q000633:toxicity; D051381:Rats; D015203:Reproducibility of Results; D014508:Urea / Q000097:blood
chemical_list: D000596:Amino Acids; D015415:Biomarkers; D001786:Blood Glucose; D014508:Urea; D009151:Mustard Gas; D005690:Galactose