[Study on the chemical constituents of Sarcandra glabra by HPLC-ESI-MS/MS].

OBJECTIVE: To study and compare the main chemical constituents of Sarcandra glabra and qingrexiaoyanning capsules which were extracted by acetic ether. METHODS: The sample solution were analyzed by a Zorbax C18 column with a gradient mobile phase composed of acetonitrile and 0.1% formic acid solution. Both UV and mass spectrometry detector were used simutaneously, full-scan detection mode was evaluated for the identification of all LC peaks. RESULTS: We analyzed the mass spectrum of every LC peak and identified 26 molecular mass from the ion chromatogram of Sarcandra glabra extraction and 16 molecular mass from the extractions of qingrexiaoyanning capsule. 5 compounds were identified. CONCLUSION: High performance liquid chromatography-mass/mass spectrometry has special advantages on analyzing the chemical constituents of traditional Chinese medicine.

[Quantitative determination of 1-deoxynojirimycin in mulberry leaves by high-performance liquid chromatographic-tandem mass/mass spectrometry].

OBJECTIVE: To develop a high-performance liquid chromatographic-tandem mass/mass spectrometric method to determine the concentration of 1-deoxynojirimycin (1-DNJ) in mulberry leaves. METHODS: 1-deoxynojirimycin was separated on an SHIMADZU HRC-NH2 column with the mobile phase consisting of acetonitrile and 0.1% formic acid. The mass spectrometric system equipped with a atmospheric pressure chemical ionization (APCI) interface was operated in Multiple Reaction Monitoring (MRM) mode. RESULTS: The retention time of 1-deoxynojirimycin was 2.87 min, and the calibration curve was linear over a concentration range from 482 microg/L to 2410 microg/L, the average recovery was 95.8%. The detection limit was 53.6 microg/L. CONCLUSION: The method is selective and sensitive for determining 1-deoxynojirimycin in mulberry leaves.

[High-performance liquid chromatography-electrospray ionization/tandem mass spectrometry of isofraxidin in Sarcandra glabra].

OBJECTIVE: To establish a method for determining isofraxidin concentrations in Sarcandra glabra and Qingrexiaoyanning capsules with high-performance liquid chromatographic-mass spectrometry. METHODS: Isofraxidin was extracted from Sarcandra glabra and Qingrexiaoyanning capsules with acetic ether and chloroform, respectively, and separated by isocratic reversed-phase chromatography. The mass spectrometric system was operated in multiple reaction monitoring mode. A pair of ions: precursor ion m/z 223 with product ion m/z 162 were chosen for the quantification of the analyte. RESULTS: The retention time of isofraxidin was 6.60 min, and the calibration curve was linear over a concentration range from 484 to 9 680 ng/ml. The average recovery was 96.7% and RSD 4.49%, with detection limit of 1 ng/ml. CONCLUSION: The method is rapid, selective and sensitive for determining isofraxidin in Sarcandra glabra and Qingrexiaoyanning capsules.

[High-performance capillary electrophoresis for determination of urinary citrate and oxalate].

OBJECTIVE: To develop a method for determining urinary citrate and oxalate using high-performance capillary electrophoresis. METHODS: Capillary electrophoresis with indirect ultraviolet (UV) detection was performed for determining urinary citrate and oxalate. Sodium hromate was used as the UV-absorbing background electrolyte. RESULTS: Citrate and oxalate had a migration time of 3.76 min and 3.14 min respectively. The calibration curves were linear within a limit of about 2 microg/ml for citrate and about 1 microg/ml for oxalate. The recovery rates of citrate and oxalate were 97.53% and 99.11% respectively. CONCLUSION: This method is simple, accurate and at low cost for determining citrate and oxalate in the urine.

[Determination of the total alkaloid content of Rhizoma coptidis in Gegenqinlian prescription].

OBJECTIVE: To determine the total content of alkaloids from Rhizoma coptidis in the traditional Chinese medicine prescription Gegenqinlian. METHODS: The extract of Gegenqinlian decoction and powder of the minipills were respectively purified with alumina column chromatography, and the total alkaloid content of Rhizoma coptidis in these preparations was determined using ultraviolet spectrophotometry at 350 nm. RESULTS: The total alkaloid content was 32.4 mg/g in the aqueous extract of Gegenqinlian decoction and 19.6 mg/g in Gegenqinlian minipills, with a recovery rate of 98.1% (RSD=2.9%). CONCLUSION: The method we employed yields accurate and stable results with much sensitivity for quality control of Gegenqinlian minipills, and also provides reference for study of Gegenqinlian prescription and other prescriptions that contain Rhizoma coptidis.

High-performance capillary electrophoresis for determining the contents of berberine, jatrorrhizine and palmatine in Gegenqinlian decoction.

OBJECTIVE: To develop a method for alkaloid isolation from the extract of Gegenqinlian decoction (a traditional Chinese herbal preparation) and content determination. METHOD: After the preparation of the Gegenqinlian decoction extract and the micropellets, the quaternary alkaloids of Coptis chinensis were isolated by high-performance capillary electrophoresis (HPCE) in a buffer solution containing 60% sodium phosphate (60 mmol/L, pH 8.0) and 40% methanol. 2-(4-hydroxyphenyl) ethylammonium chloride was used as the internal standard and the ultraviolet detection was performed at 254 nm for determining the contents of berberine, jatrorrhizine and palmatine in the extract of Gegenqinlian decoction. RESULTS: Berberine, jatrorrhizine and palmatine were successfully isolated within 6 min with recovery rates of 99.05%, 98.70% and 97.76% respectively and relative standard deviation of 2.12%, 1.85% and 1.95% respectively. CONCLUSION: HPCE is applicable for the determination and isolation of quaternary alkaloids in Coptis chinensis with high accuracy and recovery rate.