Contents of 5 components in Xingnaojing Injection were determined by UPLC-MS/MS method
[Objective]A new method for simultaneous determination of 5 index components containing curcuma dione,gemarone,L-camphor,curcumin and muscosterone in Xingnaojing Injection was established by ultra high liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).[Methods]The chromatographic column used in this research was ACQUITY HSS®T3 C18 column(2.1 mm×100 mm,1.8 μm).The mobile phase consisted of 0.1%formic acid water and 2 mmol ammonium acetate(A),methanol and 0.1%formic acid(B)with gradient elution(0 to 0.5 min,95%A;0.5 to 1.0 min,95%to 5%A;1.0 to 2.7 min,5%A;2.7 to 3.4 min,5%→95%A;3.4 to 4.0 min,95%A).The injection volume was 5 μL and the flow rate was 0.4 mL/min.The column temperature was 40℃.Electrospray ion source was adopted for positive ion monitoring,and multi-reaction monitoring mode(MRM)was used for quantitative analysis.[Results]Within 4 min,the five signature components of Xingnaojing Injection,including curcuma dione,jimarone,L-camphor,curcumin and muscatone,were completely separated.The peak area showed a good linear relationship with the concentration,and the correlation coefficient(r)was greater than 0.9980.The accuracy,repeatability and stability of the method were evaluated,and satisfactory results were obtained.The average recoveries were 98.2%to 104.2%.The contents of curcuma dione,jimarone,L-camphor,curcumin and muscatone in 6 batches of samples were 19.4 to 20.4,1.6 to 1.8,29.0 to 31.0,1.3 to 1.4,11.6 to 12.4 μg/mL,respectively.[Conclusion]The method has the advantages of high sensitivity,accuracy and reliability,and can realize the rapid detection of multiple components in Xingnaojing Injection,which provides a reference for the quality control research of this preparation.
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