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采用高效液相色谱-二极管阵列检测-电喷雾电离质谱联用技术对三物散中的八种主要化合物进行定量分析。

Quantitative analysis of the eight major compounds in the Samsoeum using a high-performance liquid chromatography coupled with diode array detection and electrospray ionization mass spectrometer.

作者信息

Weon Jin Bae, Yang Hye Jin, Lee Bohyoung, Ma Jin Yeul, Ma Choong Je

机构信息

Department of Biomaterials Engineering, Division of Bioscience and Biotechnology, Kangwon National University, Chuncheon 200-701, Korea.

TKM Converging Research Division, Korea Institute of Oriental Medicine, 483 Exporo, Yuseong-gu, Daejeon 305-811, Korea.

出版信息

Pharmacogn Mag. 2015 Apr-Jun;11(42):320-6. doi: 10.4103/0973-1296.153085.

Abstract

BACKGROUND

Samsoeum was traditionally used for treatment of a respiratory disease.

OBJECTIVE

The simultaneous determination of eight major compounds, ginsenoside Rg3, caffeic acid, puerarin, costunolide, hesperidin, naringin, glycyrrhizin, and 6-gingerol in the Samsoeum using a high-performance liquid chromatography (HPLC) coupled with diode array detection (DAD) and an electrospray ionization mass spectrometer was developed for an accurate and reliable quality assessment.

MATERIALS AND METHODS

Eight compounds were qualitative identified based on their mass spectra and by comparing with standard compounds and quantitative analyzed by HPLC-DAD. Separation of eight compounds was carried out on a LUNA C18 column (S-5 μm, 4.6 mm i.d. ×250 mm) with gradient elution composed of acetonitrile and 0.1% trifluoroacetic acid.

RESULTS

The data showed good linearity (R (2) > 0.9996). The limits of detection and the limits of quantification were <0.53 μg and 1.62 μg, respectively. Inter- and Intra-day precisions (expressed as relative standard deviation values) were within 1.94% and 1.91%, respectively. The recovery of the method was in the range of 94.24-107.90%.

CONCLUSION

The established method is effective and could be applied to quality control of Samsoeum.

摘要

背景

三所饮传统上用于治疗呼吸系统疾病。

目的

建立一种高效液相色谱(HPLC)结合二极管阵列检测(DAD)和电喷雾电离质谱法同时测定三所饮中8种主要成分人参皂苷Rg3、咖啡酸、葛根素、木香烃内酯、橙皮苷、柚皮苷、甘草酸和6-姜酚的方法,以进行准确可靠的质量评估。

材料与方法

根据质谱并与标准化合物比较对8种化合物进行定性鉴定,采用HPLC-DAD进行定量分析。8种化合物在LUNA C18柱(S-5μm,4.6mm内径×250mm)上进行分离,流动相为乙腈和0.1%三氟乙酸,采用梯度洗脱。

结果

数据显示线性关系良好(R(2)>0.9996)。检测限和定量限分别<0.53μg和1.62μg。日间和日内精密度(以相对标准偏差值表示)分别在1.94%和1.91%以内。该方法的回收率在94.24% - 107.90%范围内。

结论

所建立的方法有效,可应用于三所饮的质量控制。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9cbe/4378130/27d8083f82f3/PM-11-320-g001.jpg

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