A practical strategy for the characterization of coumarins in Radix Glehniae by liquid chromatography coupled with triple quadrupole-linear ion trap mass spectrometry.

The aim of the present study was to develop a practical method for the characterization of coumarins in Radix Glehniae by liquid chromatography-mass spectrometry (LC-MS). First, 10 coumarin standards (including two pairs of isomers) were studied, and mass spectrometry fragmentation patterns and elution time rules for the coumarins were found. Then, an extract of Radix Glehniae was analyzed by the combination of two scan modes, i.e., multiple ion monitoring-information-dependent acquisition-enhanced product ion mode (MIM-IDA-EPI) and precursor scan information-dependent acquisition-enhanced product ion mode (PREC-IDA-EPI) on a hybrid triple quadrupole-linear ion trap mass spectrometer. A total of 41 coumarins were identified on the basis of their mass spectrometry fragmentation patterns. This is the first time that these two scan modes have been combined to characterize chemical constituents in traditional Chinese medicine. This new method allowed the identification of coumarins in Radix Glehniae in trace amounts. The methodology proposed in this study could be valuable for the structural characterization of coumarins from complex natural and synthetic sources.

Simultaneous determination of ginsenosides and epimedium flavonoids in rat urine by HPLC-UV-ELSD / 中国中药杂志

<p><b>OBJECTIVE</b>To develop and validate a HPLC-UV-ELSD method for the simultaneous determination of ginsenosides and epimedium flavonoids in rat urine after intravenous administration of Jiweiling freeze-dried powder.</p><p><b>METHOD</b>Chromatographic separation was performed on a C18 HPLC column, with gradient elution of acetonitrile and water as mobile phase. An UV detector was used at detection wavelength of 220 nm. An evaporative light scattering detector (ELSD) was used at drift tube temperature of 80 degrees C and gas pressure of 172.4 kPa.</p><p><b>RESULT</b>The calibration curves were linear over the investigated concentration ranges with all correlation coefficients higher than 0.998. The a intra- and inter-day RSD were less than 9.1% and the relative errors were verage extraction recoveries for all compounds were between 88.67% and 101.2%. The within the range of -11.58% to 10.89%.</p><p><b>CONCLUSION</b>The proposed method showed appropriate accuracy and selectivity and was successfully applied to the rat urine samples analysis of saponins and flavonoids after intravenous administration of Jiweiling freeze-dried powder, which may provide some references to the apprehension of the action mechanism and clinical application.</p>

HPCE fingerprints of Forsythia suspensa from Hebei province / 中国中药杂志

<p><b>OBJECTIVE</b>To develop a HPCE analysis method for fingerprints of Forsythia suspensa from Hebei province, get reference fingerprint and compare the fingerprints of F. suspensa collected from different producing areas and different parts of the plant.</p><p><b>METHOD</b>Electrophoresis was performed on a fused silica capillary column (75 microm x 60 cm, 30 cm). The running buffer was composed of 50 mmol x L(-1) borax (adjust to pH 9.90 with 0.1 mol x L(-1) NaOH). The applied voltage was 15 kV and the temperature was 20 degrees C. The detection wavelength was 214 nm. The semblances to the crude drugs of different producing areas were compared.</p><p><b>RESULT</b>The mutual mode of HPCE fingerprints was set up with 12 common peaks. The fingerprints of F. suspensa from Hebei province had high similarity, F. suspensa from Shanxi and Henan were also of good quality. The chemical composition in different parts of the herb had big differences.</p><p><b>CONCLUSION</b>The method is simple, quick, accurate and can be used as a new means for the quality control of F. suspensa.</p>

Determination of five coumarins in radix glehniae by micellar electrokinetic capillary chromatography / 中国中药杂志

A micellar electrokinetic capillary chromatography method with ultraviolet detection was developed for the simultaneous determination of psoralen, xanthotoxin, isoimpinellin, bergapten and scopoletin in Radix Glehniae. The separation was performed on an uncoated fused silica capillary column (50.2 cm x 75 microm x 40 cm) with 20 mmol x L(-1) borax solution (pH 9.6) containing 16 mmol x L(-1) sodium dodecylsulfate (SDS) and 15% acetonitrile as running buffer at applied voltage of 22 kV. The detection wavelength was 214 nm. The effects of concentrations of borax solution, sodium dodecylsulfate (SDS), and organic modifier, voltage, temperature on the separation and sensitivity were investigated. The five active constituents were completely separated within 7 min. The linear ranges of psoralen, xanthotoxin, isoimpinellin, bergapten and scopoletin were 9.91-82.6, 37.2-162, 2.23-18.6, 2.73-22.3 and 2.89-20.1 mg x L(-1), respectively. And the average recoveries were 98.9%, 98.4%, 101.3%, 99.1% and 98.0%, respectively. This simple and rapid method provided a new basis for assessment on quality of Radix Glehniae.

Pathway and method in studies on potential basis of Chinese herbal formula / 中草药

To study the potential basis of Chinese herbal formula is very important for elucidating their compatible mechanism and promoting the modernization of Chinese materia medica. The pathway and method in studies on the potential basis of Chinese herbal formula, such as altering prescriptions, serum pharmacology, serum pharmacochemistry, fingerprints, pharmacokinetics, and metabonomics, etc. are summed up in this paper. The above-mentioned pathway and method will provide the significant basis in studying the effective components and fractions in Chinese herbal formula.

Preparation of loganin and morroniside reference substances from Fructus Corni / 中草药

Objective To establish a separation method of loganin and morroniside reference substance from Fructus Corni. Methods After extracted with hot water and precipitated with alcohol, the extract of Fructus Corni was isolated and purified by macroporous resin, silica gel column chromatography, and preparative HPLC. Loganin and morroniside were identified by UV, 1H-NMR, 13C-NMR, and MS. Results The contents of loganin and morroniside was higher than 98% by normalization method of HPLC. Conclusion The developed method is simple with lower cost, by which loganin and morroniside can be used as reference substances for the qualitative and quantitative analysis of Chinese herbal medicine.

Quality standard for Guishao Soft Capsules / 中成药

AIM: To establish the quality standard for Guishao Soft Capsules(Radix Paeoniae Alba,Radix Angelicae Sinensis,Rhizoma Chuanxiong, etc.) METHODS: Radix Paeoniae Alba,Rhizoma Atractylodis,Rhizoma Chuanxiong,Rhizoma Alismatis and Radix Angelicae Sinensis were identified by TLC.The contents of albiflorin and paeoniflorin in Guishao Soft Capsules were determined by HPLC.HPLC analytical method was carried out(using) a C_(18) column and a mixture containing 17 volume of acetonitrile and 83 volume of 0.05% acetic acid as the mobile phase.The detection wavelength was set at 230 nm. RESULTS: Spots obtained from the test solutions had the same color in reference solution and medical material in the same location,and the blank solution had no interfernece.The linear range of albiflorin was from 0.53 ?g to 1.06 ?g(r=0.999 8),the average recovery was(100.3%.) The linear range of paeoniflorin was from 0.29 ?g to 2.00 ?g(r=0.999 9),the average recovery was(99.49%.) CONCLUSION: In TLC,the spots are very clear and specific to identify the herbal medicine in Guishao Soft Capsules.It is simple,quick,high precise and accurate for HPLC to control the quality of Guishao Soft Capsules.