Chai Yifeng

Determination of ferulic acid in Angelica sinensis and Chuanxiong by capillary zone electrophoresis.

Ferulic acid in extracts of raw herbs was separated by capillary zone electrophoresis in the buffer solution of 10 mmol/L Na2B4O7. The simple and rapid method was linear, ranging from 5 to 100 µg/mL, and had a good reproducibility with the RSD below 2%. The contents of ferulic acid in Angelica sinensis and Chuanxiong could be easily determined within 15 min with no pretreatment and no interference. Copyright

The separation of anthraquinone derivatives of rhubarb by miceller electrokinetic capillary chromatography.

A micellar electrokinetic capillary chromatographic method was set up for the separation of five anthraquinone derivatives in rhubarb. Optimization of pH and sodium deoxycholate(SDC) concentrations was studied, which showed that 50 mM H3BO3-NaOH(pH 11) containing 25 mM SDC could separate the five ingredients completely within 10 min with good reproducibility of elution time.

Separation and determination of anthraquinone derivatives in rhubarb and its preparations by micellar electrokinetic capillary chromatography

A micellar electrokinetic capillary chromatographic method was set up for the quality control of rhubarb and its preparations. Anthraquinone derivatives were separated successfully within 10 min in the buffer solution of 50 mmol/L H3BO3-NaOH (pH 11) containing 25 mmol/L sodium deoxycholate. The established method, with a recovery of extraction of over 90%, has good linear relationship and reproducibility. The contents of anthraquinone derivatives in rhubarb and a tablet of Niu-huang-jie-du differed significantly, showing that the quality control of rhubarb and its preparations is necessary. Copyright

HPLC-TOF/MC in identification of chemical components in Ginseng.

Objective:To identify the chemical components in traditional Chinese herbal medicine Ginseng by high performance liquid chromatography diode array detector (HPLC-DAD) and High performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/MS).Methods: An Agilent Zorbax XDB-Cl8 column (250 mm×4.6 mm,5 μm) was used for isolation and identification of chemical components in Ginseng with a mobile phase of acetonitrile and water in gradient elution.A gradient program was used as follows:1-35 min,19% A; 35-55 min,19%-29% A; 55-70 min,29% A; 70-110 min,29%-40% A; 110-150 min,95% A.The flow rate was set at 1.0 ml/min,the injection volume was 20 μl,and the column temperature was set at 20℃.The time-of-flight mass spectrometer was equipped with an EIS ion source.Scanning mass range was between m/z 100-1 350.Results: Thirty-nine chemical compounds in Ginseng were identified unequivocally.Conclusion: Chromatographic demonstration of 39 chemical compounds of Ginseng in one run is achieved by HPLC-TOF/MS,which provides a foundation for further study on the metabolism and action mechanism of traditional Chinese herbal medicine.

HPLC-TOFMS in rapid separation and identification of chemical components in Oldenlandia diffusa and its injection preparations.

Objective To rapidly separate and identify the chemical components in traditional Chinese herbal medicine of Oldenlandia diffusa and its injection preparations by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOFMS).Methods An Agilent Zorbax XDB-Cl8 column(250 mm×4.6 mm,5 μm) was used for separation and identification of chemical components in Oldenlandia diffusa,with a mobile phase of 0.3% acetic acid(A) and methanol(B) in gradient elution,0-30 min,30%-90%B.The flow rate was set at 1.0 ml/min and the injection volume was 10 μl.The time-of-flight mass spectrometer was equipped with an EIS ion source.The scanning mass range was between m/z 100-1 000.Results The traditional Chinese medicine of Oldenlandia diffusa and its injection preparation were on-line separated and characterized by HPLC-TOFMS,and 11 chemical compounds were identified in Oldenlandia diffusa,6 compounds in market injection preparation,and 2 compounds in the injection prepared by ourselves.Conclusion Chromatographic demonstration of chemical compounds in Oldenlandia diffusa in one run provides a foundation for the further studying the metabolism and mechanism of Oldenlandia diffusa and its injection preparations.

Enantioseparation of milnacipran enantiomers and the separation mechanism on β-cyclodextrin-based chiral stationary phases by high performance liquid chromatography

建立了新型抗抑郁药米那普仑在环糊精手性固定相上的高效液相色谱拆分方法。在反相色谱条件下采用未衍生化 β -环糊精（Cyclobond I 2000）、乙酰基- β -环糊精（AC- β -CD）、2，3-二甲基- β -环糊精（DM- β -CD）、3，5-二甲基苯基氨基甲酸酯- β -环糊精（DMP- β -CD）4种手性柱分离米那普仑对映体。考察了固定相、流动相比例、pH、流速和柱温对拆分的影响。利用分子对接和结合能计算方法，研究米那普仑分子与AC- β -CD的对接过程，探讨其可能的分离机制。优化后的拆分条件如下：固定相为乙酰基- β -环糊精手性柱Astec CYCLOBOND TM I 2000 AC（25 cm×4.6 mm，5 μm），流动相为乙腈-0.1%（体积分数）pH 5.0醋酸三乙胺溶液（TEAA）（5：95，v/v），流速为0.4 mL/min，柱温为25 ℃，检测波长为220 nm。在此条件下，米那普仑对映体获得快速拆分，分离度（ R s ）为1.74，理论塔板数为10125。分子模拟结果表明引起手性识别的作用力主要是环糊精衍生化的乙酰基导致的氢键作用差异。该方法快速、高效、重现性好。