4.6 Article

Highly efficient sample preparation and quantification of constituents from traditional Chinese herbal medicines using matrix solid-phase dispersion extraction and UPLC-MS/MS

Journal

ANALYST
Volume 138, Issue 8, Pages 2279-2288

Publisher

ROYAL SOC CHEMISTRY
DOI: 10.1039/c3an36732k

Keywords

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Funding

  1. Project of the National Science & Technology Pillar Program during the Twelfth Five-year Plan Period [2012BAI29B07]
  2. National Natural Science Foundation of China [81202898]
  3. Program for the Top Doctor Innovative Talents of China Pharmaceutical University [2011BPY02]
  4. Research and Innovation Project for College Graduates of Jiangsu Province [CXZZ11-0809]

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In this work, a rapid and simple method based on matrix solid-phase dispersion (MSPD) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Guge Fengtong preparation (GGFT), a traditional Chinese herbal medicine, was investigated for validation, and eight major constituents were determined including four saponins (protodioscin, protogracillin, pseudoprotodioscin and dioscin) and four gingerols (6-gingerol, 8-gingerol, 10-gingerol and 6-shogaol). Response surface methodology and desirability function were employed to optimize the extraction conditions, such as dispersant, dispersant/sample ratio, solvent concentration, and elution volume, of MSPD. Results showed that MSPD using C-18 (1.75 g) as the dispersant material and methanol (89%, v/v) as the eluting solvent (12.00 mL) resulted in a high extraction efficiency. MSPD extraction had the advantages of combining extraction and clean-up in a single step, was less time consuming and required lower solvent volumes compared with conventional methods. Quantification of chemical compounds from GGFT preparations were performed using UPLC-MS/MS in multiple-reaction monitoring mode. The proposed method afforded a low limit of detection ranging from 0.02 to 0.40 ng for saponins and gingerols. For all the analytes, recoveries ranged from 80.9% to 103% and repeatabilities were acceptable with relative standard deviations of less than 6.81%. The proposed MSPD-UPLC-MS/MS method was successfully utilized to analyze five batches of GGFTs, and the results demonstrated that this method is simple, efficient and has potential to be applied for the quality control of herbal preparations.

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