Citation: LIU Xiao-Ting, YU Shan, YUAN Ming, GUO Qiang-Sheng, GONG Can, XU Xu. Determination of Epigoitrin in Radix Isatidis by Solid Phase Extraction-Quantitative Nuclear Magnetic Resonance Spectroscopy[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(7): 1059-1065. doi: 10.11895/j.issn.0253-3820.170115 shu

Determination of Epigoitrin in Radix Isatidis by Solid Phase Extraction-Quantitative Nuclear Magnetic Resonance Spectroscopy

School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China

Received Date: 27 February 2017
Revised Date: 26 May 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 31671928) and Natural Science Foundation of Shanghai, China (No. 15ZR1440800)

The method of quantitative nuclear magnetic resonance spectroscopy (qNMR) for determination of epigoitrin in Radix Isatidis was established based on solid phase extraction (SPE). The twice ultrasonic extraction method using pure water was used for fully extracting epigoitrin in sample, and then the extraction was enriched and concentrated by poly-Sery MCX SPE cartridge. The effect of sample pretreatment and qNMR experimental conditions was investigated. The qNMR experiment conditions were selected using DMSO as solvent, calibrated 2,3,5-triiodobenzoate as internal standard, and P₁(pulse width)=14.1 μs, d₁(pulse delay time)=5 s, N_S(number of scan)=256. The ¹H-NMR peaks of δ 5.365-5.399 (H-7b, d, 1H) of epigoitrin were chosen as the quantitative peaks. Method validation was performed including precision (intra-day precision RSD was 0.5%, and the inter-day precision was 0.8%), linearity (correlation coefficient r>0.9991), LOD (0.05 mg/g, standard curve method) and LOQ (0.19 mg/g, S/N≥150). The recoveries of the SPE-qNMR were 97.4%-101.7%. The result showed that the method was stable, accurate and reliable. With this method the epigoitrin in a real Radix Isatidis was determined to be ＜0.19-1.26 mg/g. SPE combining with qNMR could extend the application field of qNMR, especially in the detection of low-content component in complex samples.
- Quantitative nuclear magnetic resonance,
- Solid phase extraction,
- Epigoitrin,
- Radix Isatidis
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