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Journal of Chinese Pharmaceutical Sciences

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Determination of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule using quantitative nuclear magnetic resonance spectroscopy in combination with solid phase extraction

Xiaoting Liu, Jingna Xu, Kun Xiao, Qiangsheng Guo, Xu Xu*   

  1. School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China
  • Received:2020-01-12 Revised:2020-02-20 Online:2020-04-30 Published:2020-03-15
  • Contact: Tel.: +86-21-60873372, E-mail: xuxu3426@sina.com
  • Supported by:
    National Natural Science Foundation of China (Grant No. 31671928) and Natural Science Foundation of Shanghai (Grant No. 15ZR1440800).

Abstract:

The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy (qNMR) in combination with solid phase extraction (SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C18 SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and qNMR experimental conditions were investigated. The qNMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1 (pulse width) = 14.4 μs, d1 (pulse delay time) = 1 s, NS (number of scan) = 512. The 1H NMR peaks of δ 6.138–6.182 (H-8’, d, 1H) of chlorogenic acid was chosen as the quantitativepeaks. Method validation was performed, including precision (the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity (correlation coefficient r>0.9999), LOD (0.0017 mg/g) and LOQ (0.079 mg/g). The recovery of the SPE-qNMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.

Key words: Quantitative nuclear magnetic resonance spectroscopy, Solid phase extraction, Chlorogenic acid, Shuanghuanglian capsule

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