Comprehensive analysis of chemical constituents in Xingxiong injection by high performance liquid chromatography coupled with mass spectrometry / 中国天然药物

Xingxiong injection (XXI) is a widely used Chinese herbal formula prepared by the folium ginkgo extract and ligustrazine for the treatment of cardiovascular and cerebrovascular diseases. Compared with the pharmacological studies, chemical analysis and quality control studies on this formula are relatively limited. In the present study, a high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in XXI. According to the fragmentation rules and previous reports, thirty ginkgo flavonoids, four ginkgo terpene lactones, and one alkaloid were identified. A high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ MS) method was then applied to quantify ten major constituents in XXI. The method validation results indicated that the developed method had desirable specificity, linearity, precision and accuracy. The total contents of ginkgo flavonoids were about 22.05-25.51 μg·mL(-1) and the ginkgo terpene lactones amounts were about 4.41-8.70 μg·mL(-1) in six batches of XXI samples, respectively. Furthermore, cosine ratio algorithm and distance measurements were employed to evaluate the similarity of XXI samples, and the results demonstrated a high-quality consistency. This work could provide comprehensive information on the quality control of Xingxiong injection, which be helpful in the establishment of a rational quality control standard.

Study on fingerprints of astragalosides injection by HPLC-ELSD / 中国中药杂志

<p><b>OBJECTIVE</b>To develop an HPLC method for fingerprint determination of the astragalosides injection.</p><p><b>METHOD</b>Analyses were carried out at 25 degrees C on a Zorbax SB-C18 column (4.6 mm x 250 mm,5 microm). Mobile phase A was water, and B was acetonitrile. The analysis followed a linear gradient program. Initial conditions were 15% B; 0 to approximately 65 min, changed to 60% B. The flow rate was 0.8 mL x min(-1). The drift tube temparature of the ELSD was 105 degrees C, and gas flowrate was 2.7 L x min(-1).</p><p><b>RESULT</b>The RSD of relative retention time of the common peaks in the plant material, the extract and the injection fingerprints was less than 0.1%, and there was good similarity among 10 batches of samples.</p><p><b>CONCLUSION</b>The method was reliable and simple which could be used for quality control of the injection.</p>

Simultaneous determination of the major isosteroidal alkaloids and their glucosides in the bulbs of Fritillaria by high performance liquid chromatography coupled with evaporative light scattering detection / 药学学报

<p><b>AIM</b>To establish an HPLC-ELSD method for the simultaneous determination of five major bioactive isosteroidal alkaloids and gluco-alkaloids in the bulbs of Fritillaria namely peimissine, imperialine, sinpeinine A, imperialine-3 beta-glucoside and yibeinoside A.</p><p><b>METHODS</b>A Nova-Pak C18 column (150 mm x 3.9 mm ID) was used. The chromatography was carried out with a linear gradient programming. The mobile phase was acetonitrile-water (containing 0.1% diethylamine) and the flow rate was 1.0 mL.min-1.</p><p><b>RESULTS</b>The linear range of peimissine was 13.1-288.2 mg.L-1 (r2 = 0.9975), imperialine-3 beta-glucoside 7.7-169.4 mg.L-1 (r2 = 0.9993), yibeinoside A 7.3-160.6 mg.L-1 (r2 = 0.9997), imperialine 16.5-363.0 mg.L-1 (r2 = 0.9992), sinpeinine A 8.7-191.4 mg.L-1 (r2 = 0.9942).</p><p><b>CONCLUSION</b>The method is accurate with overall intra- and inter-day variation less than 5% and recovery more than 95%. The method was successfully applied to analyze five major bioactive alkaloids and gluco-alkaloids in three Fritillaria bulbs.</p>

Studies on chemical constituents of Pholidota yunnanensis / 中国中药杂志

<p><b>OBJECTIVE</b>To investigate the chemical constituents from Pholidota yunnanensis.</p><p><b>METHOD</b>Various chromatographic techniques were employed for isolation and purification of the constituents. The structures were elucidated by chemical and spectral analyses.</p><p><b>RESULT</b>Seven compounds were obtained and they were identified by spectroscopic analysis as n-nonacosane, cyclopholidone, n-dotriacontanoic acid, n-octacostyl ferulate, cyclopholidonol, cycloneolitsol and beta-sitosterol, respectively.</p><p><b>CONCLUSION</b>n-octacostyl ferulate and cycloneolitsol were isolated from genus Pholidota for the first time.</p>

Determination of epimedin C and icariin in Herba Epimedii by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To establish a RP-HPLC method for the determination of epimedin C and icariin in Herba Epimedii.</p><p><b>METHOD</b>Chromatographic conditions: Hypersil BDS-C18 column, acetonitrice and water containing 0.05% phosphoric acid as gradient eluents, G1315A photodiode array detector at 272 nm.</p><p><b>RESULT</b>The average recovery rate of epimedin C was 99.7%, RSD 1.5% (n = 9), icariin 102.5%, RSD 1.1% (n=9).</p><p><b>CONCLUSION</b>The method is reliable, stable and well repeatable. It provides the useful information for quality evaluation.</p>

Studies on the chemical constituents of Dendrobium fimbriatum / 药学学报

<p><b>AIM</b>To investigate the chemical constituents of Dendrobium fimbriatum Hook.</p><p><b>METHODS</b>Various chromatographic techniques were employed for isolation and purification of the constituents. The structures were elucidated by IR, MS, 1HNMR, 13CNMR and 2D-NMR.</p><p><b>RESULTS</b>Eight compounds were obtained and identified by spectral analysis as fimbriatone, confusarin, crepidatin, physcion, rhein, ayapin, scopolin methyl ether and n-octacostyl ferulate.</p><p><b>CONCLUSION</b>Fimbriatone is a new compound, physcion and rhein are firstly isolated from Genus Dendrobium. The others are found from this species for the first time. Fimbriatone showed potential inhibitory effects on BGC cell line.</p>

HPLC-ELSD determination of triterpenoids and triterpenoid saponins in Ilex pupurea leaves / 药学学报

<p><b>AIM</b>To establish an HPLC-ELSD method for the quantification of pedunculoside, ziyuglycoside I and rutundic acid, in the leaves of Ilex purpurea Hassk.</p><p><b>METHODS</b>By optimizing the chromatographic conditions of HPLC and the parameters of ELSD to study the methodology. Column: Allsphere ODS-2 (250 mm x 4.6 mm ID, 5 microns), mobile phase: methanol-water (59:41), flow rate: 1.0 mL.min-1, drift tube temperature: 59 degrees C, gas flow rate: 2.38 L.min-1.</p><p><b>RESULTS</b>The calibration curves were linear in the range of 2.56-25.60 micrograms for pedunculoside, 1.64-16.40 micrograms for ziyuglycoside I and 3.74-37.40 micrograms for rutundic acid. The average recovery of pedunculoside was 96.3%, RSD 1.59% (n = 5), ziyuglycoside I 97.3%, RSD 3.82% (n = 5), rutundic acid 97.7%, RSD 2.11% (n = 5). All of RSDs of the precision were less than 4% (n = 6), and the reproduciblities less than 5% (n = 6).</p><p><b>CONCLUSION</b>The method is simple, accurate, effective and feasible. It can be used for the determination of the contents of pedunculoside, ziyuglycoside I and rutundic acid in leaf of Ilex purpurea Hassk.</p>