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采用高效液相色谱-串联质谱多重反应监测模式快速同时鉴定和测定生品及炮制品山茱萸中的多种化合物。

Rapid simultaneous identification and determination of the multiple compounds in crude Fructus Corni and its processed products by HPLC-MS/MS with multiple reaction monitoring mode.

机构信息

College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, PR China.

出版信息

Pharm Biol. 2013 Mar;51(3):273-8. doi: 10.3109/13880209.2012.720689. Epub 2012 Nov 7.

Abstract

CONTEXT

Fructus Corni, a traditional Chinese medicines, is derived from the dry ripe sarcocarp of Cornus officinalis Sieb. et Zucc (Cornaceae). Gallic acid, 5-hydroxymethylfurfural, morroniside, sweroside, loganin, cornin, 7-O-methyl-morroniside and cornuside are the active constituents of Fructus Corni used in many traditional Chinese medicines. This paper describes a sensitive and specific assay for the determination of the eight bioactive compounds in crude and processed Fructus Corni extracts.

MATERIALS AND METHODS

In this paper, the eight components were determined by high performance liquid chromatography coupled with triple quadrupole mass spectrometry (MS/MS). Quantization was based on multiple reaction monitoring using the precursor production combination for determination of the eight analytes. The analysis was performed on an Agilent Zorbax Extend C(18) column (100 mm × 3.0 mm, 3.5 μm), and an electrospray ionization (ESI)-tandem interface in the positive and negative ion polarity mode was employed prior to mass spectrometric detection.

RESULTS

With the optimized conditions, the eight bioactive compounds were detected properly within 10 min. The developed method showed good precision and reproducibility with the limits of detection ranged from 0.0042 to 12.7875 ng/mL and the average recoveries ranged from 97.08 to 103.7%.

DISCUSSION AND CONCLUSION

This newly established method is validated as simple, reliable and accurate. It can be used as a valid analytical method for intrinsic quality control of crude and processed Fructus Corni.

摘要

背景

山茱萸,一种传统中药,来源于山茱萸科山茱萸的干燥成熟果肉。没食子酸、5-羟甲基糠醛、莫诺苷、獐牙菜苷、马钱苷、京尼平苷酸、7-O-甲基莫诺苷和山茱萸苷是山茱萸中用于多种中药的活性成分。本文描述了一种用于测定山茱萸生品和炮制品提取物中 8 种生物活性化合物的灵敏、特异的测定方法。

材料与方法

在本文中,采用高效液相色谱-串联三重四极杆质谱(MS/MS)法测定这 8 种成分。定量分析基于多反应监测,使用前体产物组合来测定 8 种分析物。分析采用 Agilent Zorbax Extend C(18)柱(100mm×3.0mm,3.5μm),在正、负离子极性模式下采用电喷雾电离(ESI)-串联接口进行质谱检测。

结果

采用优化条件,在 10min 内可适当检测到 8 种生物活性化合物。所建立的方法具有良好的精密度和重现性,检出限范围为 0.004212.7875ng/mL,平均回收率范围为 97.08%103.7%。

讨论与结论

新建立的方法简单、可靠、准确,可作为山茱萸生品和炮制品内在质量控制的有效分析方法。

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