Objective: To establish an UPLC-MS/MS method for the detection of Radix Bupleuri adulterated B. marginatum var. stenophyllum in Chinese patent medicine fed with whole powder, using nepasaikosaponin k, a characteristic component of B. marginatum var. stenophyllum, as an index. Methods: Agilent Eclipse Plus C18 column (100 mm×3 mm, 1.8 μm) was adopted with the mobile phase of water(A)-acetonitrile(B) in gradient mode(0-3 min, 75%A→70%A; 3-12 min, 70%A→68%A; 12-12.5 min, 68%A→10%A; 12.5-15.5 min, 10%A), the flow rate was 1.0 mL·min-1, the column temperature was 40 ℃ and the injection volume was 1 μL. The target compound was analyzed under multiple reaction monitoring(MRM) mode with an ESI- source operating in negative ion mode,m/z 943.5→797.5, m/z 943.5→781.5, m/z 943.5→635.4 were selected as the detection ion pairs. Results: The linear range of nepasaikosaponin k was 0.05-5 μg·mL-1 and r was 0.996 5, the precision RSD(n=6) of apparatus was 1.4%, the repeatability RSD(n=6) of 10% B. marginatum var. stenophyllum reference solution were 1.8%, the detection limit of adulteration was 1%. The results indicated that 2 out of 9 batches of Xiaoyao pills, 4 out of 8 batches of Jiawei Xiaoyao pills, 1 out of 10 batches of Buzhong Yiqi pills, 2 out of 10 batches of Longdan Xiegan pills contained nepasaikosaponin k exceeding the proposed limit. Conclusion: The method has been verified by methodology,is specific and sensitive, and can be applied to detect the B. marginatum var. stenophyllum which is illegally incorporated in Chinese patent medicine fed with whole powder.
CHEN Fu, HUANG Jun-zhong, LI Hua, LIU Xiao-xiao
. Study on UPLC-MS/MS method for the detection of Radix Bupleuri adulterated Bupleurum marginatum var. stenophyllum in Chinese patent medicine fed with whole powder[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(7)
: 1245
-1254
.
DOI: 10.16155/j.0254-1793.2023.07.19
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