The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutec...The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutectic mixtures of musks by solution crystallization were suggested on the basis of these phase diagrams. A new process was proposed to get musk ketone and musk xylene from the eutectics by adding acetonitrile and heptane in turn, which was verified by experiments. Musk xylene with purity of 97.50% and musk ketone with purity of 98.10% were obtained.展开更多
The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid p...The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) 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 q NMR experimental conditions were investigated. The q NMR 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 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. 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-q NMR 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.展开更多
文摘The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutectic mixtures of musks by solution crystallization were suggested on the basis of these phase diagrams. A new process was proposed to get musk ketone and musk xylene from the eutectics by adding acetonitrile and heptane in turn, which was verified by experiments. Musk xylene with purity of 97.50% and musk ketone with purity of 98.10% were obtained.
基金National Natural Science Foundation of China(Grant No.31671928)Natural Science Foundation of Shanghai(Grant No.15ZR1440800).
文摘The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) 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 q NMR experimental conditions were investigated. The q NMR 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 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. 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-q NMR 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.
