Determination of Triptolide in Kunxian Capsule by HPLC-MS Method
OBJECTIVE To establish a rapid pre-treatment and QDa determination method of triptolide in Kunxian capsule,for rapid and efficient control of product quality.METHOD A two-step sample pretreatment method was developed.The first step was to removed polar interfering components with pure water,and ethyl acetate was used as extraction reagent.The second step was to removed nonpolar flavonoid interfering components with 3％NaOH solution.The measurement method used Waters XSelect HSS T3(3.0 mm × 150 mm,2.5 μm)chromatographic column.Triptolide was determined by HPLC-QDa,with methanol(A)-0.1％formic acid aqueous solution(B)as mobile phase for gradient elution,electric spray ion source,positive ion detection,single ion monitoring(SIR)scanning mode.RESULTS The linear of triptolide was 0.137 5-17.6 μg·mL-1(r=0.999 2).RSDs of precision,repeatability,and stability(24 hours)tests were all lower than 3.0％(n=6).The average recovery rate was 90％(RSD=4.86％,n=9).The triptolide content of 17 batches of Kunxian capsules ranged from 18.58-22.09 μg/capsule,which were in line with the safe drug content limit.CONCLUSION The newly method has improved the detection efficiency by three times,reduced the use of organic solvents by about seven times,and replaced carcinogen such as 1,2-dichloroethane and chloroform with low toxic ethyl acetate,which is more suitable for continuous determination in the preparation production process,and also suitable for the study and determination of triptolide in similar preparations.
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