To ensure the quality and safety of Panax notoginseng, a method for the simultaneous determination of 10 mycotoxins in Panax notoginseng was developed using ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with acetonitrile and purified by HLB multifunction cleanup column. The separation was performed on a Phenomenex Kinetex XB-C18 column by gradient elution using methanol and 5 mmol·L(-1) ammonium acetate as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization (ESI) source operated in both positive and negative ionization modes. The linear relationships of the 10 mycotoxins were good in their respective linear ranges. The correlation coefficients (r) ranged from 0.9981 to 1.0000. The LOQs of the 10 mycotoxins were between 0.15 and 8.6 μg·kg(-1). The average recoveries ranged from 73.8% to 107.0% with relative standard deviations (RSDs) of 0.10%-10.9%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in Panax notoginseng.
Chromatography, High Pressure Liquid ; Chromatography, Liquid ; Drug Contamination ; Mycotoxins ; analysis ; Panax notoginseng ; chemistry ; Tandem Mass Spectrometry

To study the anticancer activity of griffithin from Streptocaulon griffithii Hook. f. and its effect on apoptosis of cancer cells in vitro, the inhibitory effect of griffithin on cell proliferation was studied by MTT assay, the cell apoptosis was observed by AO/EB double decoration assay and flow cytometry. Griffithin exhibited high anticancer activity on four human cancer cell lines, with IC50 ranged from 0.17 - 0.43 microg x mL(-1). Griffithin also induced apoptosis of PC-3 cells. Griffithin had anticancer activity and induced apoptosis of cancer cells.
Antineoplastic Agents, Phytogenic ; chemistry ; isolation & purification ; pharmacology ; Apocynaceae ; chemistry ; Apoptosis ; drug effects ; Cardenolides ; administration & dosage ; chemistry ; isolation & purification ; pharmacology ; Cell Cycle ; drug effects ; Cell Line, Tumor ; Cell Proliferation ; drug effects ; Cell Survival ; drug effects ; Dose-Response Relationship, Drug ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; pharmacology ; Flow Cytometry ; HL-60 Cells ; Humans ; Inhibitory Concentration 50 ; Microscopy, Fluorescence ; Molecular Structure ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry

OBJECTIVETo establish a HPLC method for simultaneous determination of 4 effective components from total flavonoids of Scutellaria barbata (FSB).

METHODSThe HPLC method was developed on an Agilent Zorbax C₁₈ column (4.6 mm × 250 mm, 5 μm). The mobile phase was composed of 1% HAc and CH₃OH:CH₃CN (80:20) with a linear gradient elution. The flow rate was 1.0 ml/min, and UV detection wave length was set at 280 nm. The column temperature was maintained at 30°C.

RESULTThe linear range of 4 effective components (scutellarin, isoscutellarein-8-O-glucuronide, isoscutellarein and luteolin) was 0.14-11.20 μg, 0.03-2.40 μg, 0.007-0.560 μg and 0.027-2.160 μg, respectively. The average recovery for 4 effective components was (101.9 ± 1.4)%, (103.5 ± 0.6)%, (98.1 ± 2.9)% and (100.5 ± 2.3)%, respectively. The contents of 4 flavonoids were determined, with scutellarin 7.3%-14.3%, isoscutellarein-8-O-glucuronide 2.4%-9.3%, isoscutellarein 0.3%-0.5%, and luteolin 0.2%-0.6%, respectively.

CONCLUSIONThe method can be used effectively to evaluate the quality of FSB.

Apigenin ; analysis ; Chromatography, High Pressure Liquid ; methods ; Flavones ; analysis ; Flavonoids ; analysis ; Glucuronates ; analysis ; Luteolin ; analysis ; Scutellaria ; chemistry

OBJECTIVETo study the stereoselectivity of R-(+) and S-(-)-propranolol glucuronidation and metabolic interaction between R(+)- and S-(-)-propranolol.

METHODSA RP-HPLC analytical method was developed for determination of R-(+)-and S-(-)-propranolol glucuronide (PG) incubated with rat hepatic microsome induced with phenobarbital (PB). The method was applied to investigate the stereoselectivity metabolism of racemic propranolol glucuronidation in vitro.

RESULTIn control and PB group, the concentration of R-(+)-PG produced at different substrates was higher than that of S-(-)-PG. Compared with the control, the V(max) and Cl(int) for R(+)-and S-(-)-propranolol increased significantly the K(m) for R(+)-propranolol was elevated, while that for S-(-) propranolol was decreased.

CONCLUSIONThere is a stereoselectivity in glucuronidation of propranolol in rat hepatic microsome induced with PB and R-(+)-propranolol is preferred. Metabolic interaction between R-(+)-and S-(-)-propranolol exists with a concentration-dependent mode.

Animals ; Enzyme Induction ; Microsomes, Liver ; enzymology ; Phenobarbital ; pharmacology ; Propranolol ; analogs & derivatives ; metabolism ; Rats ; Rats, Sprague-Dawley ; Stereoisomerism

OBJECTIVETo investigate the contents of paeoniflorin in different combination Jingzhixuefuzhuyu.

METHODUsing RP-HPLC to determine the contents of paeoniflorin in different combination Jingzhixuefuzhuyu extracts, an ODS column was used with a mobile phase of MeOH-H2O-HAC(25:75:0.15) and DAD detector at the wavelength of 230 nm.

RESULT AND CONCLUSIONDifferent combinations of Jingzhixuefu zhuyu had great influence to the contents of paeoniflorin.

Benzoates ; analysis ; Bridged-Ring Compounds ; analysis ; Bupleurum ; chemistry ; Chromatography, High Pressure Liquid ; methods ; Drug Combinations ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Glucosides ; analysis ; Monoterpenes ; Paeonia ; chemistry ; Plants, Medicinal ; chemistry

OBJECTIVETo develop a method for quality control of effective fraction in Qi-Xue-Bing-Zhi decoction, a traditional Chinese medicine (TCM).

METHODPF samples, effective fraction from Qi-Xue-Bing-Zhi decoction, were used as example, and a HPLC assay for chemical fingerprint and quantitative analysis was established.

RESULTThe contents range of Paeoniflorin (PE), Naringin (NG) and Neohesperidin (NH) in effective fractions were changed from 12.5%-16.0%, 8.4%-12.4%, 12.8%-15.3%, and their average contents were (14.7 +/- 1.1)%, (10.6 +/- 1.2)%, (14.2 +/- 0.8)% (n = 10), respectively. The fingerprints of PF samples showed 25 common peaks, and the fingerprint similarity for PF samples were all above 99.00% by comparing with the standard chromatogram.

CONCLUSIONThe method reported could be used effectively for the quality control of effective fraction from TCM.

Benzoates ; analysis ; Bridged-Ring Compounds ; analysis ; Chromatography, High Pressure Liquid ; methods ; Drug Combinations ; Drugs, Chinese Herbal ; analysis ; Flavanones ; analysis ; Glucosides ; analysis ; Hesperidin ; analogs & derivatives ; analysis ; Ligusticum ; chemistry ; Monoterpenes ; Paeonia ; chemistry ; Plants, Medicinal ; chemistry ; Quality Control ; Reproducibility of Results

OBJECTIVETo establish a quantitative analysis method for analyzing the nucleosides in Cordyceps sinensis with capillary electrophoresis, and compare the difference between natural and the cultured C. mycelia.

METHODCapillary zone electrophoresis method was employed to quantitate the adenosine, uridine, guanosine and inosine in C. sinensis, with 0.25 mg x L(-1) boric acid-sodium hydroxide buffer, pH 9.5. The working voltage was 20 kV, the temperature was 25 degrees C, and the detection wavelength was 260 nm.

RESULTWith the capillary zone electrophoresis method, the average recovery of the above 4 nucleosides was 98.9%, 95.1%, 97.8% and 98.8% respectively, with the RSD 0.4%, 1.7%, 1.3% and 5.0%. There was no adenosine in natural C. sinensis and no inosine in the cultured C. mycelia detected.

CONCLUSIONThis method can be used to determine the adenosine, uridine, guanosine and inosine in C. sinensis. The nucleosides in C. sinensis produced from Qinghai province and cultured C. mycelia are obviously different.

Adenosine ; analysis ; Animals ; Cordyceps ; chemistry ; classification ; Culture Techniques ; Electrophoresis, Capillary ; methods ; Guanosine ; analysis ; Inosine ; analysis ; Lepidoptera ; chemistry ; Uridine ; analysis

OBJECTIVETo establish a comprehensive quality control method for total flavonoid of Fructus Aurantii.

METHODSRP-HPLC and spectrophotometry were applied for the quantitative and fingerprint analysis of total flavonoid of Fructus Aurantii. The contents of naringin and neohesperidin were determined on an Agilent SB-C₁₈column (4.6 mm × 250 mm, 5 μm). The mobile phase was composed of 0.02 % H₃PO₄ and CH₃CN (80:20). The flow rate was 1 ml/min with DAD detected at 280 nm. The column temperature was maintained at 35°C. The fingerprints were developed on an Agilent SB-C₁₈ column (4.6 mm × 250 mm, 5 μm). The mobile phase was composed of 0.5 % HAc and CH₃OH with a linear gradient elution. The ratio of 0.5 % HAc and CH₃OH was: 0 min, 80:20; 10 min, 60:40; 35 min, 30:70; 50 min, 0:100. The flow rate was 1 ml/min with DAD detected at 320 nm. The column temperature was maintained at 30 degree. Meanwhile, the contents of total flavonoid were determined at 283 nm.

RESULTThe contents range of naringin, neohesperidin and total flavonoid were 38.3 %- 47.2%, 21.0 %- 28.5% and 79.9%-88.6 %, respectively. The fingerprints of the effective fractions showed 12 common peaks and the fingerprint similarity was all above 98.0 % compared with the standard chromatogram.

CONCLUSIONThe method reported in this paper can be used effectively for the quality control of total flavonoid of Fructus Aurantii.

Chromatography, High Pressure Liquid ; methods ; Citrus ; chemistry ; Flavonoids ; analysis ; Quality Control

OBJECTIVETo investigate the characteristic and influential factors of the degradation of residual pesticides and alkaloids in Radix Sophorae Flavescentis by H2O2.

METHODThe spiked samples were treated in H2O2 in different reaction time, concentration and pH value. The pesticide residuals were determined by GC-MS, and the contents of alkaloids were determined by HPLC.

RESULTH2O2 had highly activity in degrading organophosphorus and pyrethroid, but had less activity to organochlorines. The degradation processes of organophosphorus and pyrethroid followed first-order kinetics equations, and were influenced by the pH value, the concentration of H2O2 and reaction time. The contents of alkaloids in Radix Sophorae Flavescentis changed not obviously after treatment with 3 mL x L(-1) H2O2 less than 6 hours under neutral condition.

CONCLUSIONH2O2 is a useful reagent for the degradation of organophosphorus and pyrethroid in crude drug.

Alkaloids ; analysis ; Chromatography, High Pressure Liquid ; Gas Chromatography-Mass Spectrometry ; Hydrogen Peroxide ; pharmacology ; Hydrogen-Ion Concentration ; drug effects ; Organothiophosphorus Compounds ; chemistry ; Oxidation-Reduction ; drug effects ; Pesticide Residues ; chemistry ; Plants, Medicinal ; chemistry ; Pyrethrins ; chemistry ; Quinolizines ; analysis ; Sophora ; chemistry

A high performance liquid chromatography charged aerosol detector (HPLC-CAD) method was established for the simultaneous determination of five saponins (notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, Ginsenoside Rd) in Yaobitong capsule, providing a method for quality control. The sample was extracted with methanol and chromatographic separation was performed on a Waters Xbridge Phenol column (150 mm×4.6 mm, 3.5 μm) using acetonitrile-water as the mobile phase with gradient elution at a flow rate of 1.0 mL·min^-1. The column temperature was 30 ℃ and the injection volume was 10 μL. The nebulizer temperature of CAD was 35 ℃ and the air pressure was 60.2 psi, the filtration was 3.6 s, and the collection frequency was 5 Hz. Notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd showed a good linear relationship in the range of 16.96-203.5 μg·mL^-1 (R² = 0.999 3), 54.46-653.5 μg·mL^-1 (R² = 0.999 3), 10.96-131.5 μg·mL^-1 (R² = 0.999 6), 51.50-618.0 μg·mL^-1 (R² = 0.999 0), 15.94-191.3 μg·mL^-1 (R² = 0.999 4), respectively. The average recoveries were 98.96%, 100.8%, 94.76%, 100.1%, 103.1%, and RSDs were 0.87%, 1.46%, 1.85%, 2.06%, 0.96% (n = 6), respectively. The proposed method is accurate, simple and reliable, and can be used for the determination of five saponins in Yaobitong capsule.