ABSTRACT
Objective To develop a simple, rapid and sensitive method for the determination of major compounds from Gardenia jasminoides Ellis using liquid chromatography tandem mass spectrometry (LC-MS/MS).Methods The analysis was performed on Dikma Diamonsil?C18 (100mm×4.6mm, 5μm) column with acetonitrile-0.1％acetic acid and 0.1％acetic acidwater as mobile phase at a rate of 0.4ml/min.The column temperature was set at 40℃and the injection volume was 2μl.Quantification of these compounds was performed by LC-MS/MS with positive or negative ion mode electrospray ionization (ESI) in the multiple reaction monitoring (MRM) mode.Nebulizer gas, 3L/h;drying gas, 15L/h;desolvation line (DL) temperature, 240℃;heat block temperature, 300℃;CID, 230kPa.The mass transition of the precursor/product ions was monitored at m/z 391.10→149.30for shanzhiside, 573.40→365.05for genipin-1-gentiobioside, 447.30→225.15for geniposide.Results The regress equation of shanzhiside, genipin-1-gentiobioside and geniposide were Y=243.810 X-289.957, r=0.999 9;Y=137.125 X+2 092.76, r=0.999 6;Y=2 030.32 X+823 213, r=0.999 8in the range of 10.76-215.2ng/ml;516-4 128ng/ml;2 000-20 000ng/ml respectively.This validated method has good repeatability, precision, recovery and stability.The results meet the requirements by regulation.Conclusion This method shortened the analysis time and improved efficiency.It assayed the three iridoid glycosides in Gardenia jasminoides Ellis sensitively and precisely.This method can be used for the quality control of Gardenia jasminoides Ellis.
ABSTRACT
Objective: To establish a high performance liquid chromatography/mass spectrometry (HPLC-MS/MS) for the simultaneous determination of the concentration in plasma of chlorogenic acid, new chlorogenic acid, cryptochlorogenic acid, gardenia component geniposide, shanzhiside, and genipin gentian diglucoside from Lonicerae Flos in Reduning Injection iv dripped in healthy human body. Methods: Sixteen healthy subjects were iv infused of Reduning Injection with 2 ampoules, a total of 20 mL diluted with 5% glucose injection to 250 mL, iv injection time was set for 90 min, venous blood was measured at the different time points before, during, and after infusion, respectively. The conditions of determination for chlorogenic acid and other ingredients were as follows: Inertsil ODS-2 chromatographic column (150 mm × 2.1 mm, 5 μm), mobile phase (acetonitrile, 0.1% formic acid), rolling gas 137.9 kPa (20 psi), collision gas 56.16 kPa (8 psi), spray voltage -4 500 V. The LC-MS/MS conditions for determination of shanzhiside, geniposide and genipin gentian diglycoside were as follows: Ecosil C18 (150 mm × 4.6 mm, 5 μm), the mobile phase (methanol, 20 mmol/L ammonium formate, 0.1% formic acid, and 10% methanol), rolling gas 96.53 kPa (14 psi), collision gas 56.16 kPa (8 psi), spray voltage 4 500 V. Results: The tmax of neochlorogenic acid, chlorogenic acid, and cryptochlorogenic acid were 1.31, 1.38, and 144 h; Cmax were 1 241, 329 4, and 2 121 ng/mL; AUC0~t were 1 972, 5 351, and 3 596 ng·h/mL; MRT0~t were 0.708, 0.790, and 0.899 h; CL were 10.3, 385, and 5.73 L/h; Vd were 16.7, 766, and 10.7 L; t1/2 were 1.13, 1.36, and 1.27 h, respectively. The tmax of geniposide, shanzhiside, and genipin gentian diglucoside were 1.41, 1.47, and 1.47 h; Cmax were 4.49, 0.288, and 0.541 μg/mL; AUC0~t were 7.41, 0.671, and 1.22 μg·h/mL; MRT0~t were 0.856, 1.59, and 152 h; CL were 2.74, 30.0, and 16.6 L/h; Vd were 5.63, 60.9, and 35.2 L; t1/2 were 1.42, 1.42, and 1.47 h. Conclusion: The method is simple, accurate, and can be used for in vivo pharmacokinetic study on Reduning Injection.
ABSTRACT
OBJECTIVE: To establish an HPLC method for the determination of 8-O-acetyl-shanzhiside methylester in Tibet medicinal Lamiophlomis rotata.METHODS: HPLC analysis was performed on Symmetry C18(150 mm?4.6 mm,5 ?m) column with the mixture of acetonitrile-water(15∶85) served as the mobile phase.The detection wavelength was set at 234 nm.RESULTS:The linear range of 8-O-acetyl-shanzhiside methylester was 1.97～19.68 ?g?mL-1(r=0.999 6) and its average recovery was 99.53%(RSD=1.73%,n=9).CONCLUSION: The method is simple,accurate and specific,and it applies reference for quality evaluation and utilization of Tibet medicinal L.rotata.