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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneous determination of seven nucleosides and nucleobases, including adenine, uracil, adenosine, hypoxanthine, uridine, guanosine, and inosine in Inonotus obliquus samples of different batches. METHODS: Based on the mode of HPCE, uncoated fused silica capillary (75 μm × 64.5 cm, 56 cm of effective length) was used with separation voltage of 20 kV. The 55 mmol·L-1 sodium borate solution was selected as the running buffer solution (pH 9.5). The detection wavelength was set at 260 nm. The sample was injected at 5 kPa × 6 s and column temperature was maintained at 30℃. RESULTS: Good linear relationship was obtained between the response peak areas and the concentrations of all the seven nucleosides (r > 0.998 8). The average recoveries of the method were between 96.46%-102.12%. The contents of the seven nucleosides in the Inonotus obliquus samples of different origins were different. CONCLUSION: The established method is reliable, accurate, and can be used for the quality control of Inonotus obliquus.
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OBJECTIVE:To establish a method for contents determination of luteoloside,quercetin and hyperoside in Lonicera japonica. METHODS:HPCE was performed silica capillary column with detection wavelength of 360 nm and separation voltage of 20 kV,electrokinetic sampling,sampling voltage of 15 kV,sampling time of 5 s,operation temperature of 25 ℃.The buffer was consisted of 60 mmol/L sodium tetraborate-50 mmol/L natrium carbonicum-50 mmol/L hydroxypropyl-β-cyclodextrin(pH 9.2). RE-SULTS:The linear ranges of luteoloside,quercetin and hyperoside were 0.06-0.56mg/mL (r=0.9881),0.08-0.56 mg/mL (r=0.9892),0.06-0.49 mg/mL(r=0.9796),respectively. RSDs of precision,stability and reproducibility tests were all lower than 2.0%. The recoveries were 96.12%-99.77%(RSD=1.29%,n=6),95.90%-98.35%(RSD=0.89%,n=6),94.07%-97.45%(RSD=1.33%,n=6),respectively. CONCLUSIONS:The method is simple,accurate,stable and reproducible,and can be used for simultaneous determination of luteoloside,quercetin and hyperoside in L. japonica.
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OBJECTIVE: To establish a high-performance capillary electrophoresis (CE) method for determinating gallic acid in commercial Quanshen pieces of two different colors, amaranth and brownish red. METHODS: CE-UV method was used in the following condition: BGE 20 mmol·L-1 sodium borate solution, voltage 20 kV, detection wavelength 290 nm, sample injection 10 s at 5 kPa, capillary temperature room temperature. RESULTS: A quantitative method was successfully developed to determine gallic acid in Quanshen pieces within 6 min. The contents of gallic acid in 7 batches of amaranth colored Quanshen pieces were 2.70% (Hubei province), 12.08% and 7.79% (Shandong province), 2.01%, 5.78%, 6.97%, and 4.22% (Hebei province), respectively. The contents of gallic acid in brownish red colored Quanshen pieces were 1.35% (Hubei province), 1.81% and 3.42% (Shandong province), 1.87%, 3.42%, 0.44%, and 1.52% (Hebei province), respectively. CONCLUSION: The method is rapid, economical and simple and can provide a powerful quality control measure for Quanshen pieces. The contents of gallic acid in the amaranth colored Quanshen pieces are higher than those in the brownish red colored pieces.
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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneousn determination of nchlorogenic acid, caffeic acid, ferulic acid, isochlorogenic acid A, isochlorogenic acid C, neochlorogenic acid, and cynarin in the herbs of Xanthii Herba and Xanthii Fructus. METHODS: 50 mmol·L-1 borax-water was used as buffer solution (pH 9.54). The separation was performed on an uncoated fused silica capillary (64.5 cm×75 μm, 56 cm of effective length) maintained at 25℃ at voltage of 25 kV. The detection wavelength was 326 nm, and the sample was injected at 25 kPa×6 s. RESULTS: The calibration curves of the seven phenolic acid showed good linearity (r>0.9994) in the ranges of the tested concentrations, and the average recoveries of the method were between 99.85%-102.70%. CONCLUSION: The method is simple, accurate and reproducible, and can be used for the quality evaluation and control of Xanthii Herba and Xanthii Fructus.
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OBJECTIVE:To establish a method for the content determination of calceolarioside A in the Leaves of Fraxi-nus mandschurica. METHODS:HPCE was performed on the capillary of uncoated fused silica capillary,buffer solution of borate buffered saline(20 mmol/L,pH 9.3),separation voltage of 20 KV by pressure injection(injection pressure was 50 bar with 3 s), detection wavelength was 350 nm,and column temperature was 30 ℃. RESULTS:The linear range of calceolarioside A was 50-250μg/ml(r=0.999 7);RSDs of precision,stability and reproducibility tests were less than 3%,recovery was 97.48%-102.08%(RSD=1.12,n=6). CONCLUSIONS:The method is simple,good reproducibility,and can be used for the content determination of calceolarioside A in the Leaves of F. mandschurica.
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Objective: To establish a method for the determination of atractylenolide Ⅰ in Atractylodes macrocephala by HPCE. Methods:The separation conditions of HPCE were as follows:50 mmol·L-1 borate buffer was used as the running buffer, the UV de-tection was set at 210 nm, the separation voltage was 20 kV, the column temperature was 25℃ and the pressure injection was 50 mbar × 5 sec. Results:The lower detection limit was 0. 5 μg·ml-1 . The concentration of atractylenolide Ⅰ showed a linear plot within the range of 2-100 μg·ml-1(r=0. 996 0). The average recovery was 97. 1%, and the intra-and inter-day RSD was 1. 3% and 2. 5%, respectively. Conclusion:The established method is simple, sensitive and economic. The method is suitable for the quality control of atractylodes macrocephala.
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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneous determination of aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylhypaconine and benzoylmesaconine in the herbs from Aconitum plants.
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OBJECTIVE: To establish a high performance capillary electrophoresis( HPCE) method for simultaneous determination of seven nucleosides, including epigoitrin, uracil, thymine, adenosine, hypoxanthine, guanosine and uridine in Isatidis Radix. METHODS: The chromatographic separation was performed on an uncoated fused silica capillary(75 μm × 64.5 cm, 56 cm of effective length) with separation voltage of 20 kV. 60 mmol · L-1 Na2B4O7-15 mmol · L-1 β-CD was selected as the running buffer solution(pH 9.6). The detection wavelength was set at 254 nm. The sample was injected at 5 kPa × 5 s and column temperature was maintained at 25°C. RESULTS: The calibration curves of the seven nucleosides showed good linearity (r > 0.9994). The average recoveries of the method were between 97.15%-100.40%. The contents of the seven nucleosides in Isatidis Radix samples of different batches were different. CONCLUSION: The established method is simple, accurate and can be used for the quality control of Isatidis Radix.
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OBJECTIVE: To establish a micellar electrokinetic chromatography(MEKC) method for simultaneous determination of salidroside, tyrosol, ligustroflavone, specnuezhenide, oleanolic acid, and ursolic acid in Ligustri Lucidi Fructus. METHODS: 60 mmol·L-1 borax-10 mmol·L-1 SDS-30 mmol·L-1 hydroxypropyl-beta-cyclodextrin-10% methyl alcohol was used as the buffer solution (pH 9.03). Uncoated fused silica capillary (75 μm×64.5 cm, 56 cm of effective length) was used with separation voltage of 20 kV. The detection wavelength was set at 210 nm. The column temperature was maintained at 25°C, and the sample was injected at 5 kPa×6 s. RESULTS: The calibration curves of the six index components showed good linearity (r>0.95) in the range of the tested concentrations, and the average recoveries of the method were between 94.57% and 102.07% (RSD<5%). CONCLUSION: The method is simple, accurate and reproducible, and can be used for the quality control of Ligustri Lucidi Fructus.
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This study was aimed to establish a HPCE method for the content determination of hesperidin and phillyrin in Bao-He-W an (BHW). Fused silica capillary (75 cm í 50 μm) was employed and 30 mmol·L-1 borax so-lution (8% acetonitrile, pH9.64) was served as the running buffer. Other conditions were as follows: electrokinetic injection was 50 kPa í 20 s; analytical voltage was 20 kV; temperature was 20℃; and detection wavelength was 254 nm. The silica capillary was flushed with 0.1 mol·L-1 sodium hydrate and the running buffer for 10 min before each injection, respectively. The results showed that the linearity of hesperidin was in the range of 0.10~2.40 mg·mL-1 (r=0.999 4), the average recovery was 99.85% and RSD=2.34%. The phillyrin was in the range of 0.07~0.84 mg·mL-1 (r=0.999 2), the average recovery was 99.16% and RSD=2.78%. It was concluded that the method was rapid and sensitive. It can be used for the quality control of content determination of hesperidin and phillyrin in BHW.
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This study was aimed to establish a method for simultaneous determination of seven anions and organic acids in Huo-Xue Tong-Luo (HXTL) injection by HPCE. With tartaric acid as the internal standard, separation was performed on an uncoated fused silica capillary (50 μm × 64. 5 cm, 56 cm of effective length). The 14 mmol·L-1 potassium acid phthalate and 0.1 mmol·L-1 hexadecyl trimethyl ammonium chloride were selected for the running buffer solution (pH 5.6). The separation voltage was -16 kV. The detection wavelength was set at 210 nm. The column temperature was maintained at 25 ℃ . The sample was injected at 50 mbar×4 s. The results showed that calibration curves of chloride ion, sulfuric acid root ion, formate ions, malic acid, succinic acid, iodate ion and acetic acid ions showed good linear relationship 41.4-248.2 μg·mL-1 (r = 0.999 3), 12.5-74.8 μg·mL-1 (r = 0.999 8), 18.2-109.1 μg·mL-1 (r = 0.999 8), 20.3-121.6 μg·mL-1 (r = 0.999 5), 17.2-103.1 μg·mL-1 (r=0.999 1), 17.6-105.6μg·mL-1 (r=0.999 6), 51.6-309.6μg·mL-1 (r=0.999 7), respectively. The average recoveries were 102.6%, 97.3%, 102.2%, 99.0%, 99.2%, 97.8%, and 103.4%, respectively. The RSD were 1.7%, 2.0%, 1.6%, 2.6%, 2.1%, 2.9%, and 1.0%, respectively (n = 6). It was concluded that the method was accurate and reproducible. It was suitable for the determination of anions and organic acids in HXTL injection.
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OBJECTIVE: To develop an HPCE method of tetramethylpyrazine hydrochloride in rat plasma using pyramide as the internal standard. METHODS: The separation was performed on a fused-silica uncoated capillary with an inner diameter (ID) of 75 μm, an effective length of 50 cm and a total length of 60 cm. The optimum HPCE conditions were as follows: 100 mmol·L-1 SDS-30 mmol·L-1 sodium tetraborate solution (40:60) was used as the background electrolyt, the samples were injected at the anodic end at 0.5 psi for 6 s, separation voltage was 20 kV at positive power, capillary temperature was 20°C, and detection wavelength was 295 nm. RESULTS: The linear range was 1.12-286.72 mg·L-1(r=0.9996), and the inter-day and intra-day precisions expressed as RSDs were less than 4.21% and 4.74%, respectively. The average recoveries were 91.22%-97.48%, and the limit of detection was 0.16 mg·L-1. CONCLUSION: This method is rapid and accurate to quantify tetramethylpyrazine hydrochloride in rat plasma.
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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneous determination of five nucleosides and nucleobases, including adenine, adenosine, uridine, guanosine and inosine in antrodia camphorate of different batches. METHODS: Based on the mode of HPCE, uncoated fused silica capillary (75 μm×64.5 cm, 56 cm of effective length) was used with separation voltage of 22 kV. 60 mmol·L-1 sodium borate was selected for the running buffer solution (pH 9.3). The detection wavelength was set at 260 nm. The sample was injected at 50 mbar×6 s and column temperature was maintained at 28°C. RESULTS: The calibration curves of the five nucleosides showed good linearity (r>0.9995). The average recoveries of the method were between 98.83%-101.08%. The contents of the five nucleosides in Antrodia camphorate samples of different batches were different. CONCLUSION: The established method is reliable, accurate and can be used for the quality control of Antrodia camphorata.
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Objective: To develop a novel method using high-performance capillary electrophoresis coupled with DAD (HPCE-DAD) for the simultaneous determination of 10 phenolic compounds (luteolin-7-O-glucoside, rutin, quercetin-3-glucoside, quercetin-3- rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid) in Bidens bipinnata. The extraction efficiency of above mentioned compounds was compared using six different ethanol/water solutions. Methods: The effects of pH value and concentration of buffer, applied voltage, and temperature on the separation were researched. The 10 compounds were baseline separated within 16 min in a 60 cm length capillary at a separation voltage of 25 kV with a running buffer consisting of 25 mmol/L borate (pH 9.5) at wavelength of 214 nm. Results: Excellent linearities of luteolin-7-O-glucoside, rutin, quercetin-3-glucoside, quercetin-3-rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid were observed at 5.0-120, 5.0-120, 5.0-120, 5.0-120, 1.0-120, 2.5-120, 5.0-120, 2.5-120, 2.5-120, and 2.5-120 mg/L, respectively. The detection limits were at 2.5, 2.5, 2.5, 2.5, 0.5, 1.0, 2.5, 1.0, 1.0, and 1.0 mg/L, respectively. The relative standard deviations (RSD) of precision were below 5.17% (n = 6). The mean recoveries for 10 phenolic compounds in B. bipinnata ranged from 94.4% to 105.8%, with RSD values of 0.32%-4.33%. Conclusion: The contents of luteolin-7-O-glucoside, rutin, quercetin-3- glucoside, quercetin-3-rhamnoside, salicylic acid, luteolin, kaemferol, quercetin, gallic acid, and protocatechuic acid in B. bipinnata are 95.04-105.84, 78.03-110.45, 96.45-177.96, 178.78-300.00, 62.06-66.54, 71.08-72.85, 77.39-95.30, 68.27-77.43, 68.47- 88.47, and 107.24-142.43 μg/g, respectively.
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Objective To establish HPCE method for determining the mangiferin in Baihe Zhimu decoction.Methods Rutin was used as internal standard.An uncoated fused silica capillary (77 cm×75 μm,effective length of 70 cm) was served as separation gate.The electrolyte buffer was composed of 12 mmol/L borax-MeOH (90 ∶ 10).20 kV voltages were applied and detection wavelength was set at 318nm.Results Mangiferin was successfully separated within 20 rin,the linear response range was 0.06～1.14 mg/ml.The average recovery was 99.0％.Conclusion The method was simple,rapid and well reproducible.It could be used as a reliable tool for the quantity control of Baihe Zhimu decoction and descriptions containing mangiferin.
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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneous determination of catalpol, aucubin, harpagide, harpagoside, acteoside and cinnamic acid in Scrophularia ningpoensis of different batches. METHODS: 60 mmol · L-1 sodium borate was used as buffer solution (pH 9.3), uncoated fused silica capillary (64.5 cm × 75 μm id, 56 cm of effective length) was used, separation voltage was 20 kV, detection wavelength was 210 nm, column temperature was maintained at 25°C, and the sample was injected at 50 kPa, 6s. RESULTS: Six index components showed good linearity (r > 0.9971) in the range of the tested concentration, and the average recoveries of the method were between 97.05%-103.43%. CONCLUSION: The method is simple, accurate and reproducible, and can be used for quality control of Scrophularia ningpoensis. Copyright 2012 by the Chinese Pharmaceutical Association.
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OBJECTIVE: To establish a high performance capillary electrophoresis (HPCE) method for simultaneous determination of aucubin, geniposide, pinoresinol diglucoside, harpagide, and chlorogenic acid in Eucommiae Cortex. METHODS: 60 mmol·L-1 sodium borate-20 mmol·L-1 sodium dihydrogen phosphate-10% methanol was used as buffer solution (pH 10.0), un-coated fused silica capillary (64.5 cm×75 μm id, 56 cm of effective length) was used, separation voltage was 20 kV, detection wavelength was 210 nm, column temperature was maintained at 25°C, and sample was injected at 5 kPa×6 s. RESULTS: Five index components showed good linearity (r>0.9973) in the range of the tested concentration. The average recoveries of the method were between 96.63%-103.73%. CONCLUSION: The method is simple, accurate and reproducible, and can be used for quality control of Eucommiae Cortex. Copyright 2012 by the Chinese Pharmaceutical Association.
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OBJECTIVE: To establish an HPCE method for determination of N-trans-feruloyl tyramine in Lycii Fructus. METHODS: The chromatographic separation was performed on an uncoated fused silica capillary of 50 cm × 75 μm ID (40 cm of effective length). 50 mmol · L-1Na2B4O7(pH 9.0 with H3PO4) was selected as the running buffer. The applied voltage was 20 kV, and the column temperature was maintained at 25°C. The chromatogram was detected at 214 nm. RESULTS: The linearity for N-trans-feruloyl tyramine was in a range of 0.25 - 15 μg · mL-1 (r = 0.9998, n = 7). The average recovery for N-trans-feruloyl tyramine was 101.8% with RSD of 2.06%. CONCLUSION: The method is accurate, reliable, and can be used as a quality control method for N-trans-feruloyl tyramine in Lycii Fructus, which can provide basis for development and utilization of Lycii Fructus. Copyright 2012 by the Chinese Pharmaceutical Association.
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OBJECTIVE: To establish an high performance capillary electrophoresis (HPCE) method for simultaneous determination of rosmarinic acid, protocatechualdehyde, danshensu, salvanic acid B, and salvianolic acid A in Salviae Miltiorrhizae Radix et Rhizoma. And to determine the optimum drying temperature for the herb. METHODS: 10 mmol · L-1 boric acid -12 mmol · L-1 monosodium phosphate-10 mmol · L-1 SDS was used as buffer solution, an uncoated fused silica capillary column (75 μm × 64.5 cm, 56 cm of effective length) was used, the separation voltage was 18 kV, detection wavelength was 206 nm, column temperature was maintained at 20°C, and sample was injected at 5 kPa × 6 s. RESULTS: Five components showed good linearity (r>0.9990) in the ranges of the tested concentrations. The optimum drying temperature was 100°C. CONCLUSION: The method is simple, accurate and reproducible, and can be used for the quality control of Salviae Miltiorrhizae Radix et Rhizoma.
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OBJECTIVE: To establish a high performance capillary electrophoresis method with diode array detection (HPCE-DAD) method for simultaneous determination of catalpol, aucubin, geniposide, acteoside and cinnamic acid in raw and processed Rehmanniae Radix. METHODS: 60 mmol · L-1 sodium borate was used as buffer solution (5% methanol, pH 9.5), uncoated fused silica capillary (64.5 cm × 75 μm, 56 cm of effective length) was used, separation voltage was 20 kV, detection wavelength was 210 nm, column temperature was maintained at 25°C, and sample was injected at 5 kPa × 6 s. RESULTS: Five index components showed good linearity (r > 0.9978) in the ranges of the tested concentrations, the average recoveries of the method were between 97.63%-103.03%. CONCLUSION: The method is simple, accurate and reproducible, and can be used for the quality control of Rehmanniae Radix.