Latest ArticlesObjective: To establish a quantitative analysis of multi-components by single marker (QAMS) method to simultaneously determine the contents of scopolamine, anisodamine, scopolin, hyoscyamine and scopoletin in Physochlaina infundibularis Kuang. Methods: Agilent 5 TC-C18 (250 mm×4.6 mm, 5 μm) column was used with methanol-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution at a flow rate of 1.0 mL·min-1. The detection wavelengths were 210 nm and 344 nm, the column temperature was 30 °C, and the injection volume was 10 μL. The relative correction factors for scopolamine, scopolin, hyoscyamine and scopoletin and anisodamine were calculated by using anisodamine as the internal reference substance. The contents were determined and compared with the results of external standard method (ESM). Results: The five components had good linear relationship in their respective ranges(r=1.000). The relative correction factors of scopolamine, anisodamine, scopolin, hyoscyamine and scopoletin were 0.951 8, 0.562 6, 0.830 4 and 0.433 9, respectively, with good repeatability. The contents of scopolamine, anisodamine, scopolin, hyoscyamine and scopoletin in P. infundibularis from 10 habitats calculated by QAMS method were not significantly different from those determined by ESM. Conclusion: The method is accurate, stable and reproducible, and can be used for the quality control of P. infundibularis.
Objective: To investigate the source and quality of commercially available Epimedium based on HPLC fingerprint and multi-index assay, so as to provide reference for its quality evaluation and resource development. Methods: Forty batches of commercially available epimedium were collected. Fingerprint analysis and determination of the total flavonoid glycosides were performed by HPLC method. The total flavonoid glycosides were determined by UV method. And the contents of their extracts were determined. Stoichiometric analysis was employed to perform the comprehensive quality evaluation of different medicinal materials of Epimedium. Results: There were 9 different plant sources of Epimedium in the market. The five authentic Epimedium were of good quality, and the local varieties were coarse Epimedium. The contents were high in Epimedium from Hunan, while the contents were low in Epimedium from Qianling and Sichuan. The comprehensive quality ranking of Epimedium indicated that Epimedium Fletchum and Epimedium Fletchum ranked first by the principal component analysis method. The ranking of the same variety varied greatly with different habitats, and the Qianling Epimedium and adulterated Epimedium ranked last. The results of cluster analysis and principal component analysis were basically consistent. The cluster analysis showed distinguishing significance in plant sources, habitats, processing methods and contents. Based on the common pattern of E. brevicornu, a total of 8 common peaks were identified for 9 species of E. Brevicornu, and their similarities ranged from 0.066 to 0.979. Differences were observed among different species. Conclusion: Both the fingerprint similarity and the chemical model of content determination can be used to evaluate the species and quality of Epimedium.
Objective: To develop an HPLC method for determination of naphazoline hydrochloride, diphenhydram hydrochloride and lidocaine hydrochloride added in nasal cold compress gel (dew), and to establish an HPLC-triple quadrupole mass spectrometry (HPLC-MS) method to confirm the positive samples. Methods: The samples were extracted with acetonitrile, detected by high performance liquidchromatography, quantified by external standard method and confirmed by HPLC-MS. The separation was performed on a XTerra RP18 (150 mm×4.6 mm, 5 μm) column with the mobile phase consisting of 50 mmol·L-1 ammonium acetate (the pH value was adjusted to 7.8 with acetic acid or ammonia solution)-acetonitrile (72∶28) at the flow rate of 1.0 mL·min-1 and the detection wavelength was 230 nm. The analysis was performed on a BEH C18 (100 mm×2.1 mm, 1.7 μm) column with a gradient elution of 0.1% formic acid aqueous solution-0.1% formic acid acetonitrile solution. The column temperature was set at 40 ℃ and the flow rate was 0.4 mL·min-1. Electrospray ionization source was applied and operated in positive electrospray ionization and the multiple reaction monitoring mode. Results: The method showed the lowest detection concentrations of naphthazoline hydrochloride, diphenhydramine hydrochloride and lidocaine hydrochloride were 2.4 ng·mL-1, 50 ng·mL-1 and 50 ng·mL-1. The sample recoveries ranged from 93.9% to 104.6%. Good linearities were found in the concentration range of 10-200 μg·mL-1（r>0.999 0）. A total of 42 batches of samples were detected and the total positive rate was 70% (36/42). Naphthazoline hydrochloride were found in 34 batches. Diphenhydramine hydrochloride and lidocaine hydrochloride were found in 2 batches simultaneously. Conclusion: The established method is specific, sensitive, simple, accurate and reliable. It can be used for the qualitative and quantitative determination of naphthazoline hydrochloride, diphenhydramine hydrochloride and lidocaine hydrochloride in nasal cold compress gel (dew).
Objective: To establish the infrared spectrum identification model to distinguish Mingui from Angelica sinensis from other habitats. Methods: A total of 1 540 batches of A. sinensis were collected from Gansu Province through visits and field investigation, and the mid-infrared spectrum of each sample was collected by Fourier transform infrared spectroscopy. The average spectra of 423 batches of Mingui were calculated as their fingerprint. The identification threshold of Mingui was determined as 0.989 6 (μ-3σ) by mid-infrared spectroscopy combined with the “3σ” criterion. The identification model of Mingui was established. Three batches of Mingui and 97 batches of A. sinensis from other habitats were randomly selected to verify the identification model. Results: The characteristic peaks of samples were observed at 3 560, 3 389, 3 342, 2 931, 1 743, 1 650, 1 459, 1 409, 1 385, 1 374, 1 323, 1 279, 1 239, 1 128, 1 115, 1 104, 1 068, 1 053, 1 013, 1 004, 991 and 920 cm-1, etc. The mid-infrared spectra of 423 batches of Mingui were highly similar, and their peak shape, peak position and peak intensity were similar. The correlation coefficients between Mingui and the fingerprint ranged from 0.992 0 to 0.998 0. The accuracy of identification model test was 97%. Conclusion: The identification model of Mingui could be used to distinguish Mingui from other A. sinensis from other habitats.
Objective: To determine the concentration of vanillic acid by polyoxometal-based host-guest frame material modified glass carbon electrode. Methods: A stable polyacid-based host-guest metal-organic framework material PMoV@MIL-100(Fe) was synthesized by combining vanadium-substituted phosphomolybdic acid (PMoV) with MIL-100(Fe) according to the synthesis method of polyacid-based host-guest framework materials. Functional composite material PMoV@MIL-100(Fe)@Pt was prepared by composite metal nanoparticles with PMoV@MIL-100(Fe) by solution method, and was used to modify glassy carbon electrode, detect vanillic acid, and prepare vanillic acid electrochemical sensor. Results: Under optimal conditions, the vanillic acid electrochemical sensor showed wide linear range and high sensitivity. Rapid and sensitive detection of vanillic acid could be performed under mild conditions with excellent stability. Conclusion: The electrochemical sensor constructed in this experiment provides a new idea for the detection of vanillic acid.
This article focuses on the key experimental operations in the study about the applicability of microbial limit testing methods for drugs，summarizing literature and experience from the preparation of test solution，design of methods for microbial counting and control bacteria inspection，operation of microbial recovery test，bacterial liquid concentration counting，and operational methods for controlling bacterial & fungal purity. Emphasis was placed on the preparation methods of water-soluble test samples with strong antibacterial effects，non-oil and fat test samples that were not easily soluble and dispersed，and the test solution for oil and fat test samples. Detailed introduction of the sequential experimental plan for methods of aerobic bacterial count，mold & yeast count，and control bacterial inspection were introduced. Four operational methods for adding bacteria about membrane filtration were explained，and the impact of different ways of adding bacteria on the results of the method was analyzed. Summarized three counting methods for bacterial & fungal concentrations. Detailed sharing of operational experience on controlling the purity of bacterial solution. Summarized the current status about research on the applicability of microbial limit testing methods of drugs. Four suggestions for the future development of research on the applicability of microbial limit testing methods for drugs have been proposed：（1） Unify the operation about bacteria adding method in membrane filtration，scientific and reasonable；（2）Strengthen supervision of pharmaceutical production enterprises and review of microbial limit testing methods for drugs；（3）Unify the microbial limit testing methods for the drugs of the national sampling plan，and gradually collect and bind into a book；（4）Strengthen the research on the applicability of microbial limit testing methods for excipients.
To analyze the difference of chemical constituents in rhizomes and leaves of Polygonatum sibiricum from Shaanxi Province.
Ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS) was developed to determine the chemical constituents in rhizomes and leaves of Polygonatum sibiricum from Shaanxi Province. The data were analyzed by principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). The structures of chemical markers in rhizomes and leaves of Polygonatum sibiricum were identified based on accurate primary mass spectrometry and secondary mass spectrometry fragment ion，combined with the reference map，software database searching and related literature.
A total of 45 compounds were identified，there were 26 chemical ingredients with significant differences distinguished by the method of OPLS-DA，including 10 amino acids，6 flavonoids，3 organic acids，2 saccharides，1coumarin and 4 alkaloids.
The chemical markers of amino acids，organic acids and alkaloids are mainly distributed in rhizomes，and the chemical markers of flavonoids are mainly concentrated in leaves part of the plant. It is suggested that the potential multiple utilization of rhizomes and leaves of Polygonatum sibiricum from Shaanxi Province.
To establish an HPLC method for the simultaneous determination of eight components including salvianic acid A sodium，geniposidic acid，phellodendrine，salvianolic acid B，palmatine，berberine，atractylodin，tanshinone ⅡA in Shuangshi Tonglin capsules.
The determination was performed on a Capcell Pak MG Ⅱ C18 column (250 mm×4.6 mm，5 μm) with the mobile phase consisting of acetonitrile-water(containing 0.1% phosphoric acid)-water(containing 0.1% phosphoric acid and 0.2% triethylamine，pH 6.0) in a gradient mode at a flow rate of 1.0 mL·min-1. The column temperature was set at 30 ℃，the injection volume was 10 μL，and the detection wavelength was 280 nm (0-13.4 min）for salvianic acid A sodium，238 nm (13.5-17.0 min) for geniposidic acid，280 nm （17.1-51.0 min）for phellodendrine，salvianolic acid B，345 nm（51.1.1-70.0 min）for palmatine，berberine，336 nm（70.1-78.0 min）for atractylodin and 268 nm(78.1-90.0 min)for tanshinone ⅡA.
Salvianic acid A sodium，geniposidic acid，phellodendrine，salvianolic acid B，palmatine，berberine，atractylodin，tanshinoneⅡA had good linearities in their respective linear ranges with all linear correlation coefficients ≥ 0.999 5 and RSDs of the precision，repeatability and stability less than 2.0%. The average recoveries were 101.3%，98.2%，97.3%，98.1%，96.6%，97.9%，98.7%，99.6%，with RSDs lower than 2.0%. The contents of the above eight components in three batches of samples was 4.47-5.51 mg·g-1，0.93-1.44 mg·g-1，1.00-1.07 mg·g-1，5.72-8.67 mg·g-1，0.64-0.69 mg·g-1，1.62-1.90 mg·g-1，0.055-0.088 mg·g-1，0.29-0.44 mg·g-1，respectively.
The proposed method is rapid，sensitive and specific，which can be used for determination the contents of eitht components in Shuangshi Tonglin capsules.
To establish methods of thin-layer chromatography(TLC) qualitative identification and quantitative analysis of multi-components by single-marker (QAMS) according to the characterization results of the main components of Iris tectorum Maxim..
Firstly，the main components of Iris tectorum were characterized by ultra performance liquid chromatography tandem time-of-flight mass spectrometry(UPLC-Q TOF MS/MS) technology，using an ACQUITY UPLC® BEH C18 column (100 mm×2.1 mm，1.7 μm) with gradient elution using 0.1% formic acid-water (A)-acetonitrile (B) as mobile phase，and the data were collected in positive ion mode. In addition，the qualitative identification method was established by the TLC. Finally，quantitative analysis was performed on an Agilent 5 TC-C18 column (250 mm×4.6 mm，5 μm). The mobile phase was 0.05% phosphoric acid water(A)-acetonitrile(B) with gradient elution. The QAMS method was established by using tectorigenin as an internal standard to establish its relative correction factor with tectoridin and irigenin，and the contents of three isoflavones were calculated by the correction factor. At the same time，the accuracy and feasibility of the QAMS method was verified by the external standard method(ESM).
Five isoflavones were characterized (tectoridin，iristectorin B，tectorigenin，irigenin and iristectorigenin A) by UPLC-Q TOF MS/MS. A TLC identification method for four components，tectoridin，iristectorin B，tectorigenin and irigenin was established. In this study，the linearity of the three components of tectoridin，tectorigenin and irigenin were good in a certain concentration range (r>0.999)，with the average recoveries of 97.7%-100.8% and the RSDs of 1.1%-2.9%，and the relative correction factors of tectoridin and irigenin were 1.114 5 and 0.827 0，respectively. And the repeatability of the correction factors was good under different experimental conditions (RSD<5%). There was no significant difference between the contents of the three analytes in ten different batches of Iris tectorum determined by QAMS and ESM. The contents of tectorigenin，tectoridin and irigenin in 10 batches of Iris tectorum from different habitats determined by QAMS were not significantly different from those determined by ESM.
Based on the characterized components of Iris tectorum medicinal materials，the TLC and QAMS methods with high-content and stable ingredients are established. The methods are simple and stable，which can be used for qualitative and quantitative analysis and quality evaluation of Iris tectorum.
To establish the quantitative analysis of multi-components by single marker（QAMS） method to simultaneously determine the contents of rutin，hyperoside，isoquercetin and quercetin in Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati，and compare the differences in flavonoids contents.
Methanol extract of Zanthoxyli Pericarpium was analyzed on an Agilent Eclipse Plus C18 (250 mm×4.6 mm，5 μm) chromatographic column. The mobile phase was acetonitrile(A)-0.1% formic acid(B) in a gradient elution. The flow rate was 1.0 mL·min-1. The column temperature was 35 ℃，and the detection wavelength was 360 nm. The injection volume was 10 μL. Using hyperoside as the internal standard substance，the relative correction factors for the other 3 components were calculate and the flavonoids contents in Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati were determined.
The 4 components had good linear relationship within their respective ranges (r≥0.999 9). The average recovery rates of Zanthoxyli Pericarpium were 99.3%-105.1% (n=6)，while thoes of Pericarpium Zanthoxyli Armati were 91.9%-99.8% (n=6). The relative average deviations of content of Zanthoxyli Pericarpium were 0.05%-3.37%，and the relative average deviations of content of Pericarpium Zanthoxyli Armati were 0.02%-3.28%. The results obtained by QAMS method were close to those obtained by the external standard method(ESM).
This method of QAMS method is accurate and reliable. The total amount of flavonoids in Pericarpium Zanthoxyli Armati is significantly higher than that in Zanthoxyli Pericarpium. Which provides reference for the comprehensive evaluation of the quality research of Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati.
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