title: An automated dual-gradient liquid chromatography-MS/MS method for the simultaneous determination of ferulic acid, ligustrazine and ligustilide in rat plasma and its application to a pharmacokinetic study.
abstract: An automated on-line SPE and innovative fast polarity switch bioanalysis method employing dual-gradient liquid chromatography (DGLC) coupled with mass spectrometry (DGLC-MS/MS) was established and validated for the simultaneous determination of ferulic acid, ligustrazine and ligustilide in rat plasma after administration of Rhizoma Chuanxiong, Angelica sinensis extract or monomer. The proteins in plasma samples were precipitated using acetonitrile: methanol (1:1, v/v). Sulfamethoxazole was used as an internal standard. The DGLC system contains two high-pressure pumps. The first pump was used for on-line solid phase extraction with a Cyclone™ SPE column. Chromatographic separations were performed with the other pump on a Syncronis C18 rapid analytical column. The analytical column was eluted by a gradient program that featured an acetonitrile/methanol/water gradient (flow-rate, 0.4ml/min). DGLC afforded greater convenience for bioanalysis. All analytes were simultaneously monitored in positive- and negative-ion mode by SRM (selective reaction monitoring) using the fast polarity switch speed of TSQ Vantage™. Method validation of the assay was implemented. No significant matrix effect was observed. The LLOQ of all analytes were <1.0ng/ml. The precision, recovery and linearity of the analysis met the pre-established requirements. The method was applied to the pharmacokinetics of ferulic acid, ligustrazine and ligustilide in Rhizoma Chuanxiong or Angelica sinensis extracts or monomers.
authors.affiliation: Thermo Fisher Scientific, Shanghai, China.
authors.forename: Mingfei
authors.initials: M
authors.lastname: Zeng
authors.forename: Jing
authors.initials: J
authors.lastname: Zhang
authors.forename: Yifang
authors.initials: Y
authors.lastname: Yang
authors.forename: Yan
authors.initials: Y
authors.lastname: Jin
authors.forename: Wei
authors.initials: W
authors.lastname: Xiao
authors.forename: Zhenzhong
authors.initials: Z
authors.lastname: Wang
authors.forename: Gang
authors.initials: G
authors.lastname: Ding
authors.forename: Renjie
authors.initials: R
authors.lastname: Yan
mesh_terms: D015107:4-Butyrolactone / Q000031:analogs & derivatives* / Q000097:blood / Q000493:pharmacokinetics; D000042:Absorption; D000284:Administration, Oral; D000818:Animals; D001331:Automation; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D003373:Coumaric Acids / Q000097:blood* / Q000493:pharmacokinetics; D008297:Male; D008516:Medicine, Chinese Traditional; D010936:Plant Extracts / Q000032:analysis; D011312:Pressure; D011719:Pyrazines / Q000097:blood* / Q000493:pharmacokinetics; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D013420:Sulfamethoxazole / Q000737:chemistry; D053719:Tandem Mass Spectrometry
chemical_list: D003373:Coumaric Acids; D010936:Plant Extracts; D011719:Pyrazines; C027820:ligustilide; C004999:ferulic acid; D013420:Sulfamethoxazole; D015107:4-Butyrolactone; C017953:tetramethylpyrazine
keywords: DGLC; Fast polarity switching; On-line SPE; Pharmacokinetics; TSQ Vantage™