RESUMEN
To study pharmacokinetic characteristics of epimedin A, B, C and icariin after intermuscular administration of Chuankezhi injection to rat. The established RRLC-MS/MS method was applied for simultaneous determination of four analytes in rat plasma and calculating their pharmacokinetic parameters. As a result, each analyte showed a good linear relationship in the concentration range of 1-1 000 μg•L⁻¹.The intra-day precise was 96.9%-107.5% with RSD<5.99%, inter-day precise was 92.3%-105.0% with RSD<10.16%. The relative recovery of four analytes was 88.1%-101.1% with RSD<7.9% and their absolute recovery was 72.0%-86.6% with RSD<6.3%. After intermuscular administration of Chuankezhi injection, the plasma concentration of four flavonoid glycosides rapidly arose to peaks at about 10 min, and then quickly declined in rat. Tmax of epimedin A, B, C and icariin was 0.21, 0.19, 0.16 and 0.49 h, respectively, and their mean elimination half-life(t1/2z) was 0.60, 0.62, 0.47 and 0.49 h. The established method was validated to be sensitive, rapid and specific for determination of the four analytes. Serum concentration of 4 species of epimedium flavonoids in Chuankezhi injection was low, and their absorption and elimination seem quickly, displaying similar pharmacokinetic characteristics in this study.
RESUMEN
Objective]To establish a rapid resolution liquid chromatography-mass spectrometry(RRLC-MS) method for sibutramine hydrochloride, ephedrine hydrochloride and furosemide, which is the illegally added substances in diet pills. [Method]The chromatographic conditions: Agilent SB-C18 column(2.1mm×50mm, 5μm). The mobile phase consists of acetonitrile(containing 0.1% formic acid) and 0.1% formic acid solution, gradient elution with flow rate of 0.2mL·min-1; The MS conditions: electrospray ionization(ESI) source, with positive and negative ions, multiple reaction monitoring(MRM) mode to detect contents of prohibited substances in diet pills. [Result]Under the above conditions, all seven diet pills were detected with the sibutramine hydrochloride and ephedrine hydrochloride. The concentration range of the two substances was from 0.39 to 4.29μg·g-1 and from 1.63 to 8984.18μg·g-1 respectively. One drug contained furosemide, while the content was 8.71μg·g-1. [Conclusion]The method established was fast, convenient, had high sensitivity and high accuracy, which can detect prohibited substances quantitatively and qualitatively in diet pills.
RESUMEN
OBJECTIVE: To develope a method for determination of four aflatoxins (B1, B2, G1, G2) in fruit traditional Chinese medicines by rapid-resolution liquid chromatography coupled with electrospray ionization triple quadruple tandem mass spectrometry. METHODS: After being extracted with 70% methanol and purified by immunoaffinity columns, the four aflatoxins were separated on a Shim-pack XR-ODS column using gradient elution with the mobile phase of CH3CN-CH3OH-H2O mixtures monitored under MRM mode in ESI positive scan. RESULTS: There was a good linear relationship over the range of 0.102 1-10.21 ng · mL-1 for AFB1, 0.061 2-7.65 ng · mL-1 for AFB2, 0.193-9.65 ng · mL-1 for AFG1, 0.121-7.55 ng · mL-1 for AFG2 (r > 0.999 8), respectively. The average recoveries ranged from 77.0%-102.4%. CONCLUSION: This method provides a simple and feasible way to determine aflatoxins.