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Tea is a widely consumed beverage and has many important physiological properties and potential health benefits. In this study, a novel method based on supercritical fluid chromatography coupled with mass spectrometry (SFC-MS) was developed to simultaneously determine 11 amino acids in different types of tea (green teas, Oolong tea, black tea and Pu-erh tea). The separation conditions for the analysis of the selected amino acids including the column type, temperature and backpressure as well as the type of additive, were carefully optimized. The best separation of the 11 amino acids was obtained by adding water (5％, v/v) and trifluoroacetic acid (0.4％, v/v) to the organic modifier (methanol). Finally, the developed SFC-MS method was fully validated and successfully applied to the determination of these amino acids in six different tea samples. Good linearity (r ! 0.993), precision (RSDs 2.99％), accuracy (91.95％e107.09％) as well as good sample stability were observed. The limits of detection ranged from 1.42 to 14.69 ng/mL, while the limits of quantification were between 4.53 and 47.0 ng/mL. The results indicate that the contents of the 11 amino acids in the six different tea samples are greatly influenced by the degree of fermentation. The proposed SFC-MS method shows a great potential for further investi-gation of tea varieties.
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Objective: To study the protective effects and the mechanism of Salvia yunnanensis extract on hypoxia/reoxygenation injury in cultured rat H9c2 cardiomyocytes.Methods: The hypoxia/reoxygen (H/R) injury model was established in H9c2 cell strain with or without the extract of Salvia yunnanensis.The cultured H9c2 cardiomyocytes were randomly divided into 6 groups: the normal control (C) group, H/R group, H/R+verapamil (H/R+V) group, H/R+Salvia yunnanensis extract at low dose (H/R+L, 0.01 mg·L-1) group, medium dose (H/R+M, 0.1 mg·L-1) group and high dose (H/R+H, 1.0 mg·L-1) group.The cell viability was measured by MTT assay and the activity of malondialdehyde (MDA) and lactate dehydrogenase (LDH) was measured by a detection kit.Fluorescence absorbance (A) value was measured by a fluoroscopy to show the intracellular reactive oxygen species (ROS) levels.Results: Compared with that in the model group, the survival rate of myocardial cells was significantly higher in Salvia yunnanensis extract at low, medium and high dose groups (P＜0.05 or P＜0.01), and the intracellular LDH leakage (P＜0.05 or P＜0.01), the content of MDA in cytoplasm (P＜0.01) and the intracellular ROS levels significantly decreased in Salvia yunnanensis extract at high dose group (P＜0.05).Conclusion: The extract of Salvia yunnanensis has protective effect on hypoxia/reoxygenation injury in cultured rat H9c2 cardiomyocytes, and the mechanism may be related to the reduction of lipid peroxides and removal of cell oxygen free radicals.
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OBJECTIVE:To establish a method for the dissolution determination of Pentoxyverine citrate and guaifenesin tab-lets,and to compare the difference of preparations from different manufactures. METHODS:The paddle method was used to deter-mine the dissolution,using water as medium with medium volume of 1000 mL and rotation speed of 75 r/min,sampling at 45 min. HPLC method was used to determine the accumulative dissolution of pentoxyverine citrate and guaifenesin:CAPCELL PAK C18 MGⅡ S-5 column;mobile phase of acetonitrile-triethylamine phosphoric buffer solution(pH 2.6±0.05)(33:67,V/V),flow rate of 1.0 mL/min,detection wavelength of 215 nm(pentoxyverine citrate)and 275 nm(guaifenesin),column temperature of 35 ℃,sample size of 20 μL. RESULTS:The linear range of pentoxyverine citrate and guaifenesin were 5.0916-50.9155 μg/mL(r=0.9999)and 29.9995-299.9952 μg/mL(r=0.9999),respectively. RSDs of precision,stability and reproducibility tests were all lower than 2.0%. Average recoveries were 97.90%-100.68%(RSD=0.95%,n=9)and 97.09%-101.85%(RSD=1.32%,n=9). Average accu-mulative dissolution of pentoxyverine citrate in 6 manufactures of samples were 12%,98%,66%,97%,91%,32%(n=3);those of guaifenesin were 8%,95%,68%,90%,93%,18%(n=3),respectively. CONCLUSIONS:The method is simple,ac-curate,sensitive,specific and suitable for the dissolution determination of Pentoxyverine citrate and guaifenesin tablets. The dissolu-tion of samples between different manufactures and the same manufactures different batches are quite different.
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Objective:To establish an HPLC method for the simultaneous determination of rutin, salvianolic acid B and ginsen-oside Rb1 in Xinning tablets. Methods:The samples were separated on a CAPCELL PAK MG(250 mm × 4. 6 mm,5μm)column with gradient elution using acetonitrile(A) and 0. 1％ phosphoric acid(B) as the mobile phase at a flow rate of 1. 0 ml·min-1. The col-umn temperature was set at 35℃. The wavelengths were set on 354nm, 286nm and 203 nm (in a wavelength switching mode). Re-sults:The linear range of rutin was 0. 0273-1. 3600 mg·ml-1(r =1. 0000), that of salvianolic acid B was 0. 0244-1. 2200 mg· ml-1(r=1.0000),and that of ginsenoside Rb1 was 0.0186-0.9310 mg·ml-1(r=0.9999), and the average recovery (n=6) was 102.3％ (RSD=1.1％),98.7％ (RSD=0.8％) and 101.7％ (RSD=1.8％)(n=6), respectively. Conclusion: A rapid, simple, accurate HPLC method is successfully established for the simultaneous determination of 3 effective components in Xinning tab-lets, which is helpful to the quality control of Xinning tablets.
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Objective:To develop a method for the quality control of Cuochuang powder .Methods:Rhei Radix et Rhizoma, An-gelicae Dahuricae Dadix and Saposhnikoviae Radix were identified by TLC .GC was used for the determination of patchouli alcohol , menthol and borneol .Results:The TLC spots were clear without any interference from the negative control .The linear range of pat-chouli alcohol was 0.020 1-0.805 6 mg· ml-1 , that of borneol was 0.010 0-0.401 6 mg· ml-1 , and that of menthol was 0.005 1-0.202 8 mg· ml-1.The average recovery (n=6) was 102.03% (RSD=0.91%), 100.10% (RSD =1.94%) and 103.15%(RSD=1.68%),respectively.Conclusion:The method is simple, accurate and repeatable, which can be used for the quality control of Cuochuang powder .
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OBJECTIVE:To establish a method of quick identification of Fufang yuxingcao tablel(manufactured by A). METH-ODS:NIRDRS was adopted,the near-infrared diffuse reflectance spectrum were recorded by a fiber optic probe,and the conformi-ty test model was established through the consistency index (CI) value and the CI limit comparison method. The spectral range of 9 002-7 497.8 cm-1 ,6 903.8-5 596.4 cm-1 and 5 002.4-4 246.4 cm-1 was selected as the characteristic spectral band ,the spectra were preprocessed by first derivation and vector normalization with 17 smoothing points , and 7.0 was set as the CI value;the characteristic spectrum correlation coefficient model was established through the correlation coefficient method ,the spectral range of 6 200-5 500 cm-1,5 000-4 700 cm-1 was selected as the characteristic spectral band,the spectra were preprocessed by first deri-vation with 17 smoothing points,and 97% was set as the threshold. RESULTS:The above established models can rapidly identify and accurately distinguish Fufang yuxingcao tablet(manufactured by A)from similar products of other manufacturers,the CI value of the validation samples was beyond 7.0,the correlation coefficient(r)were less than 97% compared with the reference sample. CONCLUSIONS:The method is simple and rapid,and can be used for fast screening of Fufang yuxingcao tablet.
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OBJECTIVE:To establish a method for the rapid identification of Sanjiu weitai granule and quantitative analysis of moisture. METHODS:Near-infrared (NIR) spectroscopy was adopted. 38 batches of Sanjiu weitai granule were collected,NIR spectrum was determined by integrating sphere diffuse-reflectance. Conformity test model was performed by comparing consistency index(CI)value and CI limit,and quantitative model of moisture was established using partial least squares(PLS)algorithm. RE-SULTS:When CI value was less than 6,the established model can accurately distinguish Sanjiu weitai granule,the model was proven feasible;the correlation coefficient (r2) of quantitative model was 97.44,the root mean square error of cross validation (RMSECV) was 0.453,the root mean square error of prediction (RMSEP) was 0.748. CONCLUSIONS:The method is simple and rapid without destroying,which can be applied to fast screening of Sanjiu weitai granule in site and fast determination of mois-ture content.
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To study the quality of Lonicerae iaponicae flos in compound Yuxingcao tablets. Methods: HPLC-ELSD and LC-MS/MS were used to determine Lonicerae flos using macranthoidin A, macranthoside B and dipsacoside B as the control. Re-sults:HPLC-ELSD was suitable for the detection of Lonicerae flos in compound Yuxingcao tablets. LC-MS/MS was used to verify the results, which could identify the certified or counterfeit Lonicerae iaponicae flos in the samples. Conclusion:The two methods can be used to control the quality of Lonicerae iaponicae flos in compound Yuxingcao tablets.
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Infrared (IR) spectroscopy was employed to identify the Artemisinin and Piperaquine Tablets. Artemisinin and piperaquine was extracted separately by different solvents, and IR spectra were collected. IR absorption spectrum of the extract was concordant with the reference spectrum recorded in the Atlas of Infrared Spectra of Drugs, except for a group of small absorptions at 1 574 cm-1 for the artemisinin extract. It was concluded that IR method is stable and accurate, which can be used to identify the Artemisinin and Piperaquine Tablets.
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This study was aimed to establish determination method of content and related substances of piperaquine in A rtemisinin and Piperaquine Tablets, and to set the limit of related substance. HPLC was adopted on a SHISEIDO CAPCELL PAK C18 (4.6 mm í 250 mm, 5 μm) using an isocratic mobile phase consisted of acetonitrile: 0.1%trichloroaceticacid:triethylamine (18:82:0.2, V:V:V, pH 2.5) with a flow rate of 1.0 mL·min-1. The column tempera-ture was kept at 30oC and the detection wavelength was set at 216 and 237 nm, separately for the determination of related substance and content. The results showed that piperaquine and its related impurity can be separated effec-tively. The concentration-response relationship was linear over the range of 0.01-0.2 mg·mL-1 (R2=0.999 9). The av-erage recovery rate was 98.14% (RSD=0.77%, n=9). The minimum detection limit was 0.06 μg·mL-1. The solution was stable for 12 h. It was concluded that the method was specific, accurate, sensitive and suitable for the determi-nation of content and related substances of piperaquine in A rtemisinin and Piperaquine Tablets.
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A novel system was developed for the rapid determination of vitexin, vitexin-2″-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn(Crataegus pinnatifida Bge.) leaves with microemulsion liquid chromatography(MELC). The effect on the chromatography of varying the operating paramers was studied. The optimized MELC system with microemulsion was consisting of 1.0%(w/w) brij35-1.1%(w/w) n-butanol-0.1%(w/w) n-octanol-0.3%(v/v) triethylamine, the pH was adjusted to 2.5 with phosphoric acid. The type and concentration of surfactant, types of oil phase, the pH and triethylamine as the organic additive in microemulsion played an important role for separation of four flavonoids. MELC analysis was performed on a Venusil ASB C_(18) analytical column (150 mm× 4.6 mm, i.d., 5 μm). The flow rate was set at 0.8 mL/min and the eluent was detected at 340 nm for the four flavonoids. The calibration curves of the four flavonoids are linear(r>0.9995) over the concentration range of 0.95-140.0 mg/L. The mean recoveries are 98.6% to 101.6%. The results indicate that the optimized method was successfully applied to the analysis of four important flavonoids in the extract of hawthorn leaves.
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OBJECTIVE:To develop an HPLC method for determination of the content of the main compontents in haloperidol tablets. METHODS: The samples were determined on Diamonsil C18 column at a column temperature of 35 ℃. The mobile phase consisted of 0.1 mol?L-1 K2HPO4 (pH 3.0)-methanol (45∶55) at a flow rate of 1.0 mL?min-1. The UV detection wavelength was 248nm and the sample size was 20 ?L. RESULTS: The linear range for haloperidol was 0.01～1 mg?mL-1 (r=0.999 9) and its average recovery was 97.6% (RSD=1.1%). CONCLUSIONS: The method was simple, rapid, accurate and specific, and suitable for the quality control of this preparation.