ABSTRACT
Objective: To develop a GC-MS method for the simultaneous determination of six active constituents ( borneol, isoborneol, cinnamaldehyde, cinnamic acid, muscone and benzyl benzoate) in Shexiang Baoxin pills. Methods: A gas chromatogra-phy-mass spectrography (GC-MS) method was adopted using a DB-5 capillary column (30 m × 0. 25 mm,0. 1 μm). The column tem-perature was raised as the following program:the initial temperature was 70℃, maintained for 2 min, raised the temperature (5℃· min-1) to 150℃, maintained for 4 min and then raised the temperature (20℃·min-1) to 260℃, and maintained for 3 min. The range of mass-to-electric charge ratio was 10 to 425. Results:The calibration curves of borneol, isoborneol, cinnamaldehyde, cinnam-ic acid, muscone and benzyl benzoate were linear within the range of 0.022-22.000 μg·ml-1(r=0.999 6),0.024-24.000 μg· ml-1(r=0.999 6),0.028-28.000μg·ml-1(r=0.999 8),0.034-34.000μg·ml-1(r=0.999 6),0.040-40.000μg·ml-1(r=0.999 7) and 0.050-50. 000 μg·ml-1 (r =0.999 9), respectively. The average recovery was 97.20%, 97.40%, 97.53%, 99. 60%, 98. 78% and 98. 27% and RSD was 0. 89%, 1. 18%, 1. 52%, 1. 49%, 0. 79% and 1. 74%(n=6), respectively. Con-clusion:The method is accurate, suitable, convenient and reproducible, which can be used for the quality control of multi components in Shexiang Baoxin pills.
ABSTRACT
Objective:To develop a method of quantitative analysis of multi-components by single marker ( QAMS) for 4 kinds of saponins in spina date seed.Methods:Using jujuboside A as a reference, an HPLC method with a Kromasil C18 column (250 mm × 4.6 mm, 5 μm) was applied, the mobile phase was acetonitrile-0.1% phosphoric acid (30 ∶70), the flow rate was 1.0 ml · min-1 , the detection wavelength was 280 nm, the column temperature was 32℃and the injection volume was 20μl.The relative cor-rection factors among the four kinds of saponins were detected by QAMS .An external standard method was also used to determine the contents of the four saponins ( Wf ) , and the results were compared with those of QAMS ( Ws ) , and then the relative errors were calcu-lated between W f and Ws to evaluate the accuracy of QAMS , and the reproducibility was investigated as well .Results:The established QAMS was used to determine the four kinds of saponins in spina date seed , and totally 14 batches of spina date seed were determined . No significant differences were found out between the calculated values and the determined ones ( RSD<5%) .Conclusion:The vali-dated HPLC method shows the advantages of precision ,reproducibility and reliability .The established QAMS method is feasible , and suitable for the quality control of saponins in spina date seed .