Improvement of the Quality Standard of Xiangqing Zhitong Spray
Objective To improve the quality standard of Xiangqing Zhitong Spray.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify the Illicium henryi and Cynanchi Paniculati Radix et Rhizoma in the preparation.Headspace-gas chromatography(HS-GC)method was used to determine the ethanol and methanol content in the preparation.The chromatographic column was the Agilent HP-5 capillary column(30 m×0.32 mm,0.25 μm),the stationary liquid was 5%diphenyl-95%dimethyl-polysiloxane,the temperature was programmed(maintained at 40℃for 2 min,heated to 65℃at a rate of 3℃/min,then heated to 200℃at a rate of 25℃/min,and maintained for 15 min),the injector temperature was 200℃,and the detector temperature was 220℃;the headspace split injection was adopted,the headspace injection volume was 1 mL,the equilibrium temperature was 85℃,the constant temperature time was 20 min,and the split ratio was 100∶1;the quantitative ring temperature was 85℃,and the transmission line temperature was 110℃.Results The TLC chromatograms of Illicium henryi and Cynanchi Paniculati Radix et Rhizoma showed clear spots,good resolution,and there was no interference from the negative reference.The volume fractions of ethanol and methanol showed a good linear relationship with the peak area ratio of ethanol to n-propanol and methanol peak area within the range of 0.025%to 0.4%(R2 = 1.000 0)and 0.005%to 0.16%(R2 = 0.999 2)respectively.The RSDs of precision,stability and repeatability tests were no higher than 10.91%.The average recovery rates of ethanol and methanol were 104.06%and 110.00%,with the RSDs of 2.52%(n = 9)and 4.74%(n = 6).Conclusion The established method is simple,feasible,specific and stable,which can be used for the quality control of Xiangqing Zhitong Spray.
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