Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy
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Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy
Vol. 37, Issue 4, Pages: 452-458(2018)
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上海应用技术大学化学与环境工程学院
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Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy. [J]. 37(4):452-458(2018)
DOI:
Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy. [J]. 37(4):452-458(2018)DOI:
Determination of Icariin in Ruzengning Capsule by Solid Phase Extraction/Quantitative Nuclear Magnetic Resonance Spectroscopy
The quantitative nuclear magnetic resonance spectroscopy(qNMR)method for the determination of icariin in Ruzengning capsule was established based on solid phase extraction(SPE).The sample powder in capsule was ultrasonically extracted using 10%alcohol as solvent at room temperature.The extraction solution was enriched and cleaned with an HC-C18 SPE cartridge.The effects of ultrasonic extraction and SPE,qNMR experimental conditions were investigated.The qNMR experiment conditions were selected as follows:using deuterated DMSO as solvent,2,3,5-triiodobenzoate as internal standard,a P1(pulse width)of 14.1 μs,and a NS(number of scan)of 256.The 1H NMR peak of δ 7.9(2,6-H,d,2H)of icariin was chosen as the quantitative peak.Method validation was performed with the intra-day RSD of 0.43%and the inter-day RSD of 0.75%.The linear correlation coefficient(r)was 0.999 9 between the peak area ratio and mass ratio of icariin to internal standard.LOD was 0.122 mg/g and LOQ was 0.368 mg/g.The recoveries of the SPE-qNMR were in the range of 99.8%-103.0%.The result showed that the method was stable,accurate and reliabile.With no need of icariin standard,the method was applied in the determination of icariin in 3 batches of real Ruzengning capsule.
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定量核磁共振波谱法固相萃取淫羊藿苷乳增宁胶囊
Keywords
quantitative nuclear magnetic resonancesolid phase extractionicariinRuzengning capsule
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