ABSTRACT
Objective:To develop a method of quantitative analysis of multi-components by single marker( QAMS) for nine kinds of alkaloids in Xiaohuoluo pills. Methods: An HPLC-QTOF-MS method with an Agilent ZORBAX Extend-C18 RRHT(2. 1 mm × 50 mm,1. 8 μm) column was applied. The flow rate was 0. 21 ml·min-1 . The column temperature was 30 ℃. The mobile phase was methanol (A)-water (B;containing 0. 1％ formic acid and 2. 5 mmol·L-1 ammonium acetate) with gradient elution. The aconitine was used as the internal standard, and the relative correction factor ( RCFs) of hypaconitine, mesaconitine, benzoylaconine, benzoyl-hypaconine, benzoylmesaconine, aconine, hypaconine and mesaconine was respectively established, and the reproducibility inspection on the RCF was performed. The contents of the other 8 kinds of aconitum alkaloids were calculated according to the RCF. At the same time, an external standard method ( ESM) was performed for the content determination of the nine alkaloids. The results of the two methods were compared. The feasibility and accuracy of the QAMS method were verified. Results:Within a certain range,the RCF of hypacontine,mesacontine, benzoylaconine, benzoylhypaconine, benzoyl mesaconine, aconine, hypaconine and mesaconine to aconitine was 1. 736,1. 979,1. 0471,0. 9242,1. 2901,1. 3078,1. 2859,and 1. 0948,respectively. The QAMS method was established for determi-ning alkaloids. There were no significant differences between the results of the QAMS method and those of the external standard method ( ESM) . Conclusion:With the validation of methodology, the method established in our study can be used for the content determina-tion of aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylhypaconine, benzoylmesaconine, aconine, hypaconine and mesaconine in xiaohuoluo pills.
ABSTRACT
Objective:To determine the content of lead, cadmium, arsenic, mercury and copper in Xiaohuoluo pills produced by 34 enterprises. Methods:Using microwave digestion, the contents of lead, cadmium and arsenic were determined by graphite furnace atomic absorption spectrometry;the content of mercury was determined by hydride generation atomic absorption spectrophotometry;the content of copper was determined by air-acetylene flame atomic absorption. Results: Lead, cadmium, arsenic and mercury in Xiao-huoluo pills from 34 different manufacturers were beyond the limits in various degrees. Conclusion: The method is simple and accu-rate, and can be used in the heavy metal determination of Xiaohuoluo pills.
ABSTRACT
AIM:To establish a capillary electrophoresis with field-amplified sample stacking method for the separation and determination of aconitine alkaloid in Xiaohuoluo Pills. METHODS: An uncoated fused-silica capi-llary column(50 ?m i.d.?43 cm,effective length 35 cm) was used.The running buffer was 60 mmol/L phosphate electrolyte solution(pH=6.0)-acetonitrile(8(∶)2).The ruuning voltage was 10 kV and the capillary inlet was dipped in water for 5 s with 3.5 kPa prior to electrokinetic injection(12 kV,30 s).The detection wavelength was 235 nm. RESULTS: This method allowed 400 fold enrichment of aconitine alkaloid.A good linear relation was obtained in the range of 37.5～2.4?10~3 ng/mL (r=0.999 5),with the detection limit of 9.4 ng/mL.The average recovery was 97.6% with the RSD of 1.9%. CONCLUSION: The method is simple,rapid,specific and selective with high stacking efficiency;it provides a new reliable means for production and quality control of Xiaohuoluo Pills.