通关藤饮片中两种特异性C21甾体皂苷含量测定方法的建立OA
Establishment of content determination method for two specific C21-steroid saponins in Marsdenia tenacissima decoction pieces
目的 建立通关藤饮片中两种特异性C21甾体皂苷——11-O-异丁酰基-12-O-乙酰基通关藤苷元B-3-O-茯苓二糖基(化合物T)与17β-通关藤苷元B的含量测定方法.方法 采用超高效液相色谱-串联质谱联用法(UPLC-MS/MS),用XSelect HSS T3 XP色谱柱,以0.1%甲酸水-甲醇为流动相进行梯度洗脱,流速为0.3 mL/min,进样量为5 μL,柱温为40℃;质谱采用电喷雾离子源,以多反应监测模式进行正/负离子采集.结果 化合物T和17β-通关藤苷元B的质量浓度分别在10～200、20～200 ng/mL范围内与峰面积呈良好线性关系,r分别为0.993 1、0.998 6;精密度、重复性、准确度及稳定性的RSD均小于4.5%(n=5～6);在3批饮片中的含量分别为94.0～102.8、1 705.4～1 736.2 μg/g.结论 所建立的方法可用于通关藤饮片中上述两种特异性C21甾体皂苷的含量测定.
OBJECTIVE To establish a content determination method for two specific C21-steroid saponins namely 3-O-β-allopyranosyl-(1→4)-β-oleandropyranosyl-11-O-isobutyryl-12-O-acetyl tenacigenin B(compound T)and 17β-tenacigenin B in Marsdenia tenacissima decoction pieces.METHODS Ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was adopted.An XSelect HSS T3 XP chromatographic column was used.Gradient elution was performed with 0.1%formic acid aqueous solution-methanol as the mobile phase.The flow rate was 0.3 mL/min,the injection volume was 5 μL,and the column temperature was 40℃.An electrospray ionization source was applied for mass spectrometry,and multiple reaction monitoring mode was used for positive-and negative-ion acquisition.RESULTS The linear relationships of compound T and 17β-tenacigenin B were good within the concentration ranges of 10-200 ng/mL and 20-200 ng/mL,with r values of 0.993 1 and 0.998 6,respectively;the RSD values of precision,repeatability,accuracy,and stability were all below 4.5%(n=5-6).Their contents in three batches of decoction pieces were 94.0-102.8 μg/g and 1 705.4-1 736.2 μg/g,respectively.CONCLUSIONS The established method can be applied for the content determination of the two specific C21-steroid saponins mentioned above in M.tenacissima decoction pieces.
王祁民;鞠倩;范理菊;李颖;马银玲;董占军
河北省人民医院药学部,石家庄 050051河北省人民医院药学部,石家庄 050051河北省人民医院药学部,石家庄 050051||河北省临床药学重点实验室,石家庄 050051河北省人民医院药学部,石家庄 050051||河北省临床药学重点实验室,石家庄 050051河北省人民医院药学部,石家庄 050051||河北省临床药学重点实验室,石家庄 050051河北省人民医院药学部,石家庄 050051||河北省临床药学重点实验室,石家庄 050051
医药卫生
通关藤11-O-异丁酰基-12-O-乙酰基通关藤苷元B-3-O-茯苓二糖基17β-通关藤苷元B含量测定
Marsdenia tenacissima3-O-β-allopyranosyl-(1→4)-β-oleandropyranosyl-11-O-isobutyryl-12-O-acetyl tenacigenin B17β-tenacigenin Bcontent determination
《中国药房》 2026 (17)
2254-2257,4
国家自然科学基金项目(No.82104286)河北省自然科学基金项目(No.H2020307043)河北省医学科学研究课题(No.20230353)
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