Simultaneous determination of 9-dehydro-17-hydro-andrographolide and sodium 9-dehydro-17-hydro-andrographolide-19-yl sulfate in rat plasma by UHPLC-ESI-MS/MS after administration of xiyanping injection: application to a pharmacokinetic study.
9-Dehydro-17-hydro-andrographolide (DHA) and sodium 9-dehydro-17-hydro-andrographolide-19-yl sulfate (DHAS) are active ingredients of xiyanping injection in clinical use. A simple, rapid and sensitive UHPLC-ESI-MS/MS method was developed for the determination of DHA and DHAS in rat plasma, and the pharmacokinetics of DHA and DHAS after intravenous administration of xiyanping injection was investigated. The plasma samples were treated with methanol to precipitate out protein, and the separation of DHA and DHAS was achieved on a Waters BEH C18 column with a mobile phase consisting of acetonitrile and 10 mmol/L ammonium acetate solution at a flow rate of 0.4 mL/min. DHA, DHAS and the internal standard (internal standard, IS) diethylstilbestrol were detected at negative ion mode. The precursor-product ion pairs used in multiple reaction monitoring mode were: m/z 349.1 → 286.9 (DHA), m/z 428.9 → 96.0 (DHAS) and m/z 267.1 → 236.9 (IS). Calibration curves offered satisfactory linearity within the test range, and all correlation coefficients were >0.995. The lower limit of detection of DHA and DHAS in plasma samples were determined to be 0.1 ng/mL. The lower limit of quantitation was 0.5 ng/mL for DHA and DHAS. All the recoveries of the quality control samples were in the range of 86.0-102.4%. The ratios of matrix effect were between 89.2 and 105.1%. The method was fully validated and successfully applied to the pharmacokinetic study of DHA and DHAS in rats. The study showed that both DHA and DHAS were distributed and eliminated rapidly in rats.
Jiangxi Institute for Drug and Food Control, Nanchang, 330029, People's Republic of China.
Lan
L
Chong
Weikang
W
Chen
Yuehua
Y
Luo
Zihua
Z
Jiang
D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004054:Diethylstilbestrol; D004224:Diterpenes / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D057230:Limit of Detection; D016014:Linear Models; D008297:Male; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013431:Sulfates / Q000097:blood / Q000737:chemistry / Q000493:pharmacokinetics; D013463:Sulfuric Acid Esters / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D053719:Tandem Mass Spectrometry / Q000379:methods*
C587544:9-dehydro-17-hydro-andrographolide-19-yl sulfuric acid; D004224:Diterpenes; D013431:Sulfates; D013463:Sulfuric Acid Esters; C030419:andrographolide; D004054:Diethylstilbestrol