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1.
Article in Chinese | WPRIM | ID: wpr-879037

ABSTRACT

Chrysanthemum is widely used as a type of edible flower and also considered as the important materials of many beverages in China. Due to the occurrence of diseases and pests, and the lack of regulations for species, frequency, dose of pesticides in Chrysanthemum, pesticides have become one of the main pollutants in Chrysanthemum. The pesticide residues in Chrysanthemum were detected frequently and worth noting. This paper focused on the types of pesticides, pesticide residue detection techniques, and risk assessment methods for Chrysanthemums on the basis of relevant literatures. The pesticide residues of traditional Chinese medicine are mainly organochlorines, organophosphorus and pyrethroids, and the detection techniques include gas chromatography(GC), liquid chromatography(LC) or both combined with mass spectrometry(MS). With the increasing use of traditional Chinese medicine, Chrysanthemum is widely circulated in the market. Therefore, it is important to understand the current situation of pesticide residues in different varieties of Chrysanthemum, so as to provide theoretical reference for the control of quality and safety of Chrysanthemum and the formulation of the maximum residue limit.


Subject(s)
China , Chromatography, Liquid , Chrysanthemum/genetics , Gas Chromatography-Mass Spectrometry , Pesticide Residues/analysis
2.
Article in Chinese | WPRIM | ID: wpr-878986

ABSTRACT

This paper aims to solve the problems of complicated-unstable test solution preparation process and insufficient extraction of the active ingredient astragaloside Ⅳ in the legal method for the determination of astragaloside Ⅳ in Astragali Radix. The continuous single-factor analysis of seven main factors affecting the content of astragaloside Ⅳ was carried out by HPLC-ELSD, and then the pre-paration method of test solution was optimized. This optimized method exhibited excellent performance in precision, repeatability and stability. The average recovery rate of astragaloside Ⅳ was 99.65% with RSD 2.2%. Astragaloside Ⅳ showed a good linearity between the logarithm of peak area and the logarithm of injection quantity in the range of 0.46-9.1 μg(r=0.999 6). The contents of astragaloside Ⅳ in 29 batches of Astragali Radix were determined by the new and the legal methods. The results showed that the average content of astragaloside Ⅳ in these Astragali Radix samples determined by the former method was 1.458 times than that of the latter one, indicating the new method was simple, reliable and more adequate to extract target compound. According to the results, it is suggested to improve the content standard of astragaloside Ⅳ in Astragali Radix in the new edition of Chinese Pharmacopeia.


Subject(s)
Astragalus Plant , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Saponins , Triterpenes/analysis
3.
Article in Chinese | WPRIM | ID: wpr-827975

ABSTRACT

Taking Lonicerae Japonicae Flos as an example, the method of "expert consensus of different regions" was used to screen the representative samples and evaluate their commodity grades. The correlation analysis, hierarchical cluster analysis and partial least squares discriminant analysis(PLS-DA) of "commodity grade-appearance characteristic-component content" were carried out to reveal the scientificity of traditional commodity grade of Chinese medicinal material. By referring to the existing literature and the grade investigation from the sample collection regions, 78 "initial grade" samples were screened out from 118 collected samples. Authoritative experts from four regions(n=4) including Linyi(Shangdong province), Bozhou(Anhui province), Anguo(Hebei province) and Beijing were organized to evaluate their commodity grades, separately. Based on the grade consistency rate(R_i≥70%), 69 "local grade" samples were screened out from the "initial grade" samples. Based on the average grade consistency rate ■ "authoritative grade" samples were screened out from the "local grade" samples, including15 first-grade samples, 9 second-grade samples, 11 third-grade samples and 17 fourth-grade samples. For these "authoritative grade" samples, the main appea-rance characteristics were quantified and the contents of 13 components were determined by ultra performance liquid chromatography(UPLC). Furthermore, the total contents of 6 phenolic acids, 4 flavonoids and 3 iridoids were calculated, respectively. The results of correlation analysis showed that 4 appearance characteristics indices were correlated with the commodity grades: color, rate of yellow bars(including blooming flowers), rate of black heads(including black bars), and rate of stems and leaves(including bud debris). Five component content indices were correlated with the commodity grades: chlorogenic acid, isochlorogenic acid C, sweroside, loganin and the total contents of six phenolic acids. Furthermore, chlorogenic acid, loganin and the total contents of six phenolic acids showed significantly negative correlation with the main appearance characteristics, indicating that the appearance characteristics of Lonicerae Japonicae Flos can reflect its internal quality, and these 3 indices can be used as quality markers(Q-markers). The results of hierarchical cluster analysis showed that the samples of four grades were classified into four categories, and the samples with the same grades and the same categories accounted for 80.8% of the total samples, while the samples with the different grades were obviously classified into different categories. The results of PLS-DA analysis showed that the samples of different grades showed obvious intragroup aggregation and intergroup dispersion. The above results indicated that it was feasible to evaluate the traditional commodity grade of Lonicerae Japonicae Flos by the method of "expert consensus of different regions". For the evaluation of traditional commodity grade of Chinese medicinal material, the samples should be representative, expert conclusions should have enough consensuses, and grade determination should be authoritative. As the crystallization of clinical experience, traditional commodity grade can scientifically reflect the internal quality of Chinese medicinal material.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Flowers , Lonicera , Quality Control
4.
Article in Chinese | WPRIM | ID: wpr-774546

ABSTRACT

HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used 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 20 μL. The experimental data were analyzed by the SPSS 22.0 and GraphPad Prism 7.0. The established triterpenoids fingerprints were specific, and the 10 components were well separated and showed good linearity(r≥0.999 6) within the concentration ranges tested. The mean recoveries were between 98.53%-103.8%(RSD 1.7%-2.7%). The method was specific and repeatable, and could be used for identification and quality evaluation of Poria. The results showed that the contents of 10 triterpenoids were positively correlated with each other. The contents of 10 triterpenoids of samples collected from producing areas were higher than that collected from markets. The total contents of 10 triterpenoids of samples collected from Hubei and Yunnan province were slightly higher than that from Anhui province, but the contents of samples from Anhui province were varied in smaller ranges.


Subject(s)
China , Chromatography, High Pressure Liquid , Materia Medica , Poria , Chemistry
5.
Article in Chinese | WPRIM | ID: wpr-774514

ABSTRACT

In order to improve the quality control level of Ligustri Lucidi Fructus(LLF) and to explore the changes of chemical components after processing,the HPLC method for fingerprint and simultaneous determination of the major polar components in LLF were established. The octadecylsilane bonded silica gel was used as the stationary phase,with acetonitrile as the mobile phase A and0. 2% formic acid as the mobile phase B in a gradient elution procedure at a flow rate of 1. 0 m L·min-1. The detection wavelength was set at 280 nm and the column temperature was 25 ℃. There were 22 common peaks,20 of which were selected from the fingerprint of LLF and its wine-steamed product,respectively,and 14 chromatographic peaks were identified with reference substances. With the same chromatographic conditions,seven components were quantitatively analyzed and the results of system adaptability and methodology investigation all met the requirements of content determination. Compared with the crude LLF,the content of 5-hydroxymethyl furfural and salidroside significantly increased in wine-steamed LLF,while the contents of iridoid glycosides generally decreased. The method provided a basis for quality control of LLF and its processed products as well as the related preparations.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Chemistry , Fruit , Chemistry , Furaldehyde , Glucosides , Iridoid Glycosides , Ligustrum , Chemistry , Phenols , Phytochemicals
6.
Article in Chinese | WPRIM | ID: wpr-773186

ABSTRACT

Due to lack of reference substances,the content of triterpenoid saponins in traditional Chinese medicines is usually characterized by colorimetric determination of total saponins. However,the specificity of colorimetric method is poor,and the determination result is not accurate enough. So,in this paper,the content determination method of total triterpenoid saponins was studied by taking Akebiae Caulis saponins as an example. The contents of three main saponin aglycones,including arjunolic acid,hederagenin and oleanolic acid,were determined by HPLC method. Referring to the content determination method of total flavonol glycosides in Ginkgo biloba leaves in the 2015 edition of Chinese Pharmacopoeia,the content of Akebiae Caulis saponins was obtained by multiplying the total content of the three above-mentioned aglycones with conversion coefficient. LC-MS/MS analysis results showed that mutongsaponin C and aponin PJIwere the two main triterpene saponins in Akebiae Caulis,and they shared the same molecular formula. So,the average value of the ratios of the molecular weight between mutongsaponin C and the three aglycones was defined as the conversion coefficient.The three aglycones were separated on an ACE Excel 3 C18-AR column( 4. 6 mm×150 mm,3 μm),and methanol-water( containing0. 04% glacial acetic acid and 0. 02% triethylamine) was used as mobile phase with gradient elution. The detection wavelength was set at 210 nm,and the flow rate was 0. 5 m L·min-1. The results showed that there was a good linearity among the ranges of 1. 053-16. 84,0. 200-3. 200 and 1. 515-24. 24 μg for arjunolic acid,hederagenin and oleanolic acid,respectively. Their average recoveries were97. 90%,97. 50% and 100. 5%,with RSD of 2. 0%,2. 9% and 2. 9%,respectively. The results of methodological investigation met the requirements of content determination. The conversion coefficient was 2. 31. This method is simple and reliable,and can be used for the determination of total triterpenoid saponins in Akebiae Caulis. The assay strategy can be used for the determination of total triterpenoid saponins in other traditional Chinese medicines.


Subject(s)
Chromatography, High Pressure Liquid , Chromatography, Liquid , Drugs, Chinese Herbal , Medicine, Chinese Traditional , Phytochemicals , Ranunculales , Chemistry , Saponins , Tandem Mass Spectrometry , Triterpenes
7.
Article in Chinese | WPRIM | ID: wpr-773151

ABSTRACT

To search for the active diuretic fractions of Clematidis Armandii Caulis( CAC) and determine its main active chemical components by using liquid chromatography-mass spectrometry( LC-MS) and diuretic activity evaluation. CAC 75% ethanol extracts and extracts from different polar solvents were orally administered to saline-loaded rats at different doses. 6 h urinary volume,p H and contents of electrolyte Na+,K+and Cl-were measured. The chemical components of the active fractions were separated and identified by ultra performance liquid chromatography-electrospray ionization-quadrupole time of flight-mass spectrometry( UPLC-ESI-Q-TOF-MS/MS) method. As compared with the control group,the urine volume was increased by 44%( P< 0. 01) and 34%( P < 0. 05) in CAC75% ethanol extract 57. 74 and 28. 8 mg·kg-1 groups respectively; the Na+excretion was increased by 52%( P< 0. 01) and 45%( P<0. 05),respectively; while the Cl-excretion was increased by 101%( P<0. 01) and 85%( P<0. 05),respectively. The urine volume,Na+excretion and Cl-excretion were increased by 50%( P< 0. 01),58%( P< 0. 05),and 65%( P< 0. 05) respectively in petroleum ether extract 70. 98 mg·kg-1 group as compared with the control group. While for the n-butanol extract 194. 18 mg·kg-1 group,the urine volume,Na+and Cl-excretion were increased by 42%( P<0. 01),41%( P<0. 05) and 97%( P<0. 01),respectively. The diuretic activity of other fractions was not obvious. There was no statistical difference in K+excretion in all groups. The results of LC-MS analysis showed that six compounds,including two sterols,one chromogen and three fatty acids,were identified from petroleum ether extract.Fourteen compounds,including six triterpenoid saponins,six lignin glycosides,one sterol glycoside and one phenolic glycoside,were identified from the n-butanol extract. All the results suggested that the ethanol extract of CAC had remarkable diuretic activity and its main effective components included sterol,triterpenoid saponin and lignin glycosides.


Subject(s)
Animals , Ascomycota , Chemistry , Diuretics , Pharmacology , Materia Medica , Pharmacology , Rats , Solvents , Spectrometry, Mass, Electrospray Ionization , Tandem Mass Spectrometry
8.
Article in Chinese | WPRIM | ID: wpr-773128

ABSTRACT

To construct a quality management model for the whole industry chain of compound Danshen Tablets,and quality control system for all key links in the production of compound Danshen Tablets. In this paper,with salvianolic acid B as internal reference substance,three batches of mix standards were prepared,and three sets of relative correlation factors between salvianolic acid B and other phenolic acids were calculated in parallel. Finally,the correlation factors are obtained on average. The quality transfer process was studied by optimizing the concentration of Salvia miltiorrhiza extract. The results showed that RSD among three sets of relative correlation factors ranged between 1. 7%-4. 1%,with no significant difference between the quantitative result of two methods. In addition,the quality transfer study showed that with the rise of the concentration temperature,the content of phenolic acid components changed,which had a significant effect on the salvianolic acid B at more than 80 ℃. It was suggested to rationally control the concentration temperature during the industrial production. The results of this study provide a methodology for the establishment of the quality control system for the whole industry chain of compound Danshen Tablets,and quality control methods for the improvement of the quality of medicinal materials and finished medicine products.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Chemistry , Hydroxybenzoates , Quality Control , Salvia miltiorrhiza , Chemistry , Tablets
9.
Article in Chinese | WPRIM | ID: wpr-777501

ABSTRACT

To solve the problems of the poor resolution of chromatographic separation,the weak durability of the relative correction factors,and the low accuracy of content determination results in the quantitative analysis of multi-components by single-marker( QAMS) method with andrographolide as the internal reference substance in the existing research of Andrographis Herba,a new QAMS method using dehydroandrographolide as the internal reference substance was established for the first time in this study. This new method can be used to simultaneously determine four diterpene lactones,including andrographolide( A),neoandrographolide( B),14-deoxyandrographolide( C),and dehydroandrographolide( S) through the optimization of chromatographic conditions and systematic investigation of methodology. At the present HPLC chromatographic conditions,four components could be well separated( R > 1. 5),and the methodology validations could satisfy the requirement of quantitative analysis. The relative correction factors( RCFs) of fA/S,fB/S,fC/S were determined as 0. 65,0. 54,0. 78,respectively. The relative standard deviations( RSDs) of their RCFs ranged between 1. 3%-5. 1%,0. 25%-0. 33%,0. 070%-0. 15%,0. 070%-0. 22%,respectively with three brands of HPLC instruments,five brands of C18 column,different flow rates( 0. 9,1. 0,1. 1 m L·min~(-1)),and different column temperatures( 25,30,35 ℃),indicating good durability of the RCFs. The relative retention value( RRV) method was used to locate the chromatographic peak of the components to be determined.The RRVs of rA/S,rB/S,and rC/Swere 0. 44,0. 86,0. 97,respectively. The RSDs of the RRVs ranged between 0. 030%-1. 6% with different HPLC instruments and columns,showing accurate peak location. The present QAMS method and the external standard method( ESM)were both used to determine the contents of four diterpene lactones from Andrographis Herba( 6 batches of medicinal materials and 18 batches of cut crude drugs). The relative errors of the determined content results between two methods were less than 2. 0%. It demonstrated that there was no significant difference in content results between these two methods,indicating good accuracy of the present QAMS method. Therefore,in this study,an accurate and highly durable QAMS method using dehydroandrographolide as the internal reference substance was established for simultaneous determination of four diterpene lactones. This method could be used to effectively control the quality of Andrographis Herba and provide technical basis for the formulation of traditional Chinese medicine industry standard and improvement of the Chinese Pharmacopoeia standard of Andrographis Herba.


Subject(s)
Andrographis , Chromatography, High Pressure Liquid , Diterpenes , Drugs, Chinese Herbal , Quality Control
10.
Article in Chinese | WPRIM | ID: wpr-771559

ABSTRACT

To investigate the dynamic change law of the main components in Ligustri Lucidi Fructus during the wine-steaming process and attempt to establish the characteristic quality standard of wine-steamed Ligustri Lucidi Fructus by determining the content of salidroside and specnuezhenide using Ultra Performance Liquid Chromatography (UPLC) technology at different processing time points (12, 15, 18, 21, 24 h). The chromatographic separation was performed on Waters Acquity UPLC®BEH C₁₈ column (2.1 mm×50 mm, 1.7 μm) with acetonitrile and 0.2% formic acid aqueous solution as the mobile phase for gradient elution; and the detection wavelength was set at 280 nm; the flow rate was 0.5 mL·min⁻¹, and the column temperature was set at 40 °C. The results showed that the two components were well separated in the above conditions. The salidroside and specnuezhenide showed a good linear relationship within the range of 10.19-326 ng and 49.53-1 585 ng, respectively. Their average recovery was 103.4% and 101.7% with RSD of 0.81% and 0.79%, respectively. With the extension of processing time, the content of specnuezhenide was decreased, while salidroside was gradually increased. For the 27 batches of Ligustri Lucidi Fructus, the content of salidroside was between 0.042 5% and 0.192 4%, and that of specnuezhenide was between 0.829 7% and 5.218 0%. While for the 25 batches of wine-steamed Ligustri Lucidi Fructus, the content of the first one was between 0.229 2% and 1.045 8%, and the latter one was between 0.743 8% and 3.645 4%. As compared with Ligustri Lucidi Fructus, the ratio of specnuezhenide to salidroside was significantly decreased in the wine-steamed Ligustri Lucidi Fructus. According to the experimental results, the quality standard of Ligustri Lucidi Fructus is tentatively fixed as follows: the content of specnuezhenide shall not be less than 0.80%, and the ratio of specnuezhenide content/salidroside content (Sp/Sa) should not be smaller than 15. As for the wine-steamed ones, the content of salidroside should not be less than 0.20%, and specnuezhenide content should not be less than 0.70%; Sp/Sa should not be greater than 8. The method established in this study is simple and reliable, which could be used for the content detection of salidroside and specnuezhenide in Ligustri Lucidi Fructus samples. The characteristic quality standard established in this study could be used to distinguish the Ligustri Lucidi Fructus and wine-steamed Ligustri Lucidi Fructus.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Fruit , Ligustrum , Wine
11.
Article in Chinese | WPRIM | ID: wpr-776412

ABSTRACT

A quantitative nuclear magnetic resonance method(qNMR) was established for determination of the absolute content of febrifugine. Proton nuclear magnetic resonance spectroscopy of febrifugine was obtained in DMSO-d₆ with hydroquinone as the internal standard substance on a Bruker Ascend 600 MHz superconducting nuclear resonance spectrometer at 298 K. The specific parameters were as follows: the observing frequency was 600 MHz,spectra width was 7 211 Hz, pulse width was 9.70 μs, pulse sequence was zg30,scan times was 32 and relaxation time was 2 s. The proton signal peaked at δ 7.71 for febrifugine and δ 6.55 for hydroquinone were selected as the quantification peaks. Linear regression of quantitative peak area ratio of febrifugine-hydroquinone versus their mass ratio yielded a correlation coefficient of 0.999 6 and a regression equation of +0.008 6.The linear range of febrifugine was 2.17-17.07 g·L⁻¹,the precision RSD was 0.78%(=6),the repeatability RSD was 1.2%(=6),and the contents of three batches of febrifugine sample were 94.91%,95.09% and 95.52%,respectively. The content of febrifugine was 96.44% determined by high performance liquid chromatography(HPLC). The relative error of the content of febrigugine determinted by qNMR and HPLC methods was 1.27%. The results showed that the internal standard method of proton nuclear magnetic resonance spectroscopy could be used to determine the absolute content of febrifugine.


Subject(s)
Magnetic Resonance Spectroscopy , Piperidines , Protons , Quinazolines
12.
Article in Chinese | WPRIM | ID: wpr-256048

ABSTRACT

To prepare Cinnamomi Ramulus pieces standard decoction and establish its quality standard, provide quality reference for formula granules and other clinic non-traditional forms of medicines, and lay a foundation for standard decoction research for the pieces containing essential oil. 14 batches of Cinnamomi Ramulus pieces with different quality were collected from market and their extraction process was further improved based on the preparation principle of standard decoction to prepare the standard decoction of Cinnamomi Ramulus pieces. Then its transfer rate of Cinnamaldehyde, dry extract rate and pH value were calculated to evaluate its process stability; and a method for chromatographic fingerprint and content determination was also established. Results revealed that the dry extract rate for standard decoction of Cinnamomi Ramulus pieces was from 6.06%-8.95%, with an average value of 7.18%; the transfer rate of cinnamaldehyde was at the range of 29.6%-54.3%, with an average of 43.2%; and the pH value was at the range of 4.33-4.82. The fingerprint similarities between 14 batches of standard decoction of Cinnmomi Rammulus pieces and reference fingerprint were all>0.9. The established method for standard decoction was stable and its quality standard was perfect, suitable for evaluating the quality of standard decoction of Cinnanomi Ramulus pieces.

13.
Article in Chinese | WPRIM | ID: wpr-350123

ABSTRACT

To develop the HPLC method for simultaneous determination of febrifugine and isofebrifugine in Dichroa febrifuga root, and on the basis of this, the feasibility of quantitative analysis of multi-component by a single-marker (QAMS) model for the determination of the two alkaloids was investigated. The chromatographic separation was performed on an octadecyl bonded silica gel column with mixed solvent consisting of acetonitrile-water-glacial acetic acid-triethylamine (9∶91∶0.36∶0.745) as mobile phase at a flow rate of 1.0 mL•min⁻¹. The detection wavelength was set at 225 nm, and the column temperature was set at 30 ℃. The linear range of febrifugine and isofebrifugine were 10.7-426 ng and 10.6-424 ng, respectively. Their average recovery were 98.33% (RSD 2.7%) and 100.4% (RSD 1.8%), respectively. On the basis of this established method, febrifugine was used as the internal reference substance to calculate the relative correction factors (RCF) and the relative retention values (RRV) of isofebrifugine to febrifugine. Through a series of methodology evaluations, the two alkaloids were simultaneously assayed only by quantitative determination of febrifugine. This result played the part of demonstration role for the application of QAMS model in the determination of isomers.

14.
Article in Chinese | WPRIM | ID: wpr-335877

ABSTRACT

To investigate the stability and degradation kinetics of febrifugine. The results showed that within 24 hours, febrifugine content was decreased by only 1% in mobile phase solvent, but its content was decreased to be 90% of the initial content in the water, methanol, 50% methanol and 10% acetonitrile solution. When the pH value of the solution was between 3 and 7, the retention rate of febrifugine in 24 hours was over 98%, but its content was decreased by about 12% in alkaline solution (pH 9.0). The higher the temperature, the worse the stability of febrifugine. At 40-80 ℃, the content of febrifugine was decreased to be 60% of its initial content in 10 hours, but the content was decreased by only 5% in 10 h at 20 ℃.However, no matter 40 ℃or 60 ℃, febrifugine was mainly transformed into isofebrifugine, and the total content of febrifugine and isofebrifugine was equal to their initial total content in 10 hours, while incase of 80 ℃, the total content was decreased to be 83.33% in 10 h, which suggested that the structure of febrifugine was absolutely changed, not just isomerized to be isofebrigugine at high temperature. Light had a significant impact on the stability of febrifugine. Under bright light, the content of febrifugine was reduced by about 23% in 108 h, but it only decreased by about 10% in the natural light or darkness. In artificial gastric fluid (pH 1.4) and artificial intestinal fluid (pH 6.8), the content of febrifugine was decreased by less than 5% in 10 h. After storage at high temperature(60 ℃), high humidity [(75±1)%] and strong light (3 000 lx) conditions for 10 d, the content of solid febrifugine was decreased by 0.27%, 7.6% and 5.39%, respectively. The degradation of febrifugine basically complied with the first-order reaction kinetic process in the following conditions: in water, methanol, 50%methanol and 10% acetonitrile solvents, alkaline solution (pH>7), different light intensity and different temperatures (20,40 ℃). Therefore, no matter the isolation and purification of febrifugine or the production of the related preparations, it should be done fast in the acidic solution, low temperature and dark conditions, while the febrifugine solid should be kept in dry and dark conditions.

15.
Article in Chinese | WPRIM | ID: wpr-335758

ABSTRACT

An UPLC method was developed for the studies of fingerprint and quantification of multi-components for Evodiae Fructus. The chromatographic separation was performed on a C₁₈ column (2.1 mm×50 mm,1.7 μm) with mobile phase of 0.2% formic acid-acetonitrile and 0.2% formic acid-water in gradient mode, and the detection wavelength was set at 320 nm.Dehydroevodiamine was used as the reference peak, there were 24 common peaks in the fingerprint of 29 samples were detected, and among them 10 chromatographic peaks were identified with the reference substance and they were neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, hyperin, isorhamnetin-3-O-β-D-rutinoside, dehydroevodiamine, evodiamine, rutaecarpine, evocarpine and dihydroevocarpine. The fingerprint data was evaluated with similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine (Version 2008A), and the similarity of 19 batches of Evodiae Fructus was greater than 0.9 in the 29 samples. In addition, 9 components including neochlorogenic acid, chlorogenic acid, hyperin, isorhamnetin-3-O-β-D-rutinoside, dehydroevodiamine, evodiamine, rutaecarpine, evocarpine and dihydroevocarpine were simultaneously determined at the same chromatographic conditions, whose peak area integral values showed good linear relationship at the range of 0.000 46-0.138, 0.000 146-0.175, 0.000 412-0.124, 0.000 448-0.134, 0.000 452-0.136, 0.003 38-0.169, 0.000 44-0.132, 0.001 07-0.128, 0.001 71-0.128, respectively. Their average recoveries were 100.3%, 100.4%, 101.6%, 97.51%, 102.9%, 101.4%, 103.8%, 104.0%, 95.99%, and RSD were 2.4%, 2.0%, 3.0%, 0.80%, 1.9%, 2.1%, 1.1%, 2.2%, 2.4%, respectively. The established UPLC method not only realized the full separation of all chemical constituents of Evodiae Fructus within 20 minutes, but also achieved the chromatographic fingerprint determination and simultaneous multi-components determination of Evodiae Fructus at the same chromatographic conditions. Compared with other methods in literatures, the method has the following characteristics of strong specificity, good separation, high purity of chromatographic peaks, simplity and feasibility, which provides better means for the simultaneous qualitative and quantitative analysis of Evodiae Fructus.

16.
Article in Chinese | WPRIM | ID: wpr-231010

ABSTRACT

In this study, an HPLC method was developed for simultaneous determination of seven alkaloids (cytosine, oxymatrine, N-oxysophocarpine, N-methylcytisine, sophoranol, matrine, and sophocarpine) and three flavonoids (trifolirhizin, fermononetin, and maackiain) from different samples of Sophorae Tonkinensis Radix et Rhizoma. Samples were analyzed on a Welch XtimateTM C₁₈ column (4. 6 mm× 250 mm, 5 μm) eluted with the mobile phase of acetonitrile (A) and 0.01 mol•L⁻¹ ammonium acetate solution (pH 8.0) (B) in a linear gradient mode as follows: 0-20 min,4%-14% A;20-30 min,14%-25% A;30-45 min,25%-40% A;45-65 min,40%-55% A;65-75 min,55% A. The flow rate of the mobile phase, the column temperature, and the PDA detector wavelength were set at 1.0 mL•min⁻¹, 30 ℃, and 225 nm, respectively. For the method validation, these ten compounds showed good separation and satisfactory linearity (r≥0.999 7) within the concentration ranges tested. The mean recoveries were in the range of 98.60% to 102.6% with the RSD (n=6) between 0.60% and 3.7%. This method was proved to be simple, accurate and repeatable. The quantitative results showed that there were significant differences in the contents of seven alkaloids and three flavonoids among the different samples. This result revealed that the quality of Sophorae Tonkinensis Radix et Rhizoma varied widely. This method could be used for the simultaneous determination of the multi-ingredients from Sophorae Tonkinensis Radix et Rhizoma, which might provide scientific evidences to evaluate/control the quality of Sophorae Tonkinensis Radix et Rhizoma, comprehensively.

17.
Article in Chinese | WPRIM | ID: wpr-279194

ABSTRACT

To establish and analyze the HPLC specific chromatograms of Xingnaojing injection manufactured by different factories. The separation was performed on a Thermo BDS Hypersil C₁₈ column (4.6 mm×250 mm, 5 μm), with the mobile phase consisting of acetonitrile-0.02% formic acid aqueous solution for gradient elution. The flow rate was 1.0 mL•min⁻¹, and the column temperature was 35 ℃. The detection wavelength was set at 254 nm, and the sample size was 20 μL. Eleven chromatographic peaks were identified as characteristic peaks of HPLC specific chromatograms of Xingnaojing injection, after analyzing 29 batches of Xingnaojing injection samples. Compared with the reference substances, seven of them were identified as eucarvone, camphor, curcumenone, curcumenol, curdione, curzerenone and germacrone, respectively. HPLC specific chromatograms of Xingnaojing injection manufactured by three factories could be easily classified into three categories after investigation with computer-aided similarity evaluation system combined with principal component analysis. The established HPLC specific chromatograms provide a basis for scientific evaluation and effective control of the quality of Xingnaojing injection.

18.
Article in Chinese | WPRIM | ID: wpr-272737

ABSTRACT

A new method based on ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of 22 endocannabinoids(eCBs) and relevant compounds in ovariectomized rat plasma. After being extracted by solid-phase column(SPE), the plasma samples were detected by using UPLC-MS/MS. Analysis was carried out with ACQUITY UPLC BEH C₁₈ column. The mobile phase was 0.1% acetic acid solution(A)-acetonitrile and isopropanol(9∶1, B) for the gradient elution. In the positive ion multiple reaction monitoring(MRM) mode, deuterated reagents were taken as standard alternatives to calculate recoveries and simultaneously quantify 22 endocannabinoids. The established method provided a good linearity for the 22 eCBs, and their linearly dependent coefficients were all higher than 0.99. The limits of quantitation(LOQs) ranged from 0.089 6 to 1.965 2 nmol•L-1. Relative recoveries of 5 deuterated surrogates ranged between 11.40% and 129.9%. The repeatability study results showed that RSD was all less than 8.0%. The established method could be used to analyze PGF2a EA, AEA and other endogenous cannabinoids in plasma samples of ovariectomized rats. In summary, this method was proved to boast a high sensitivity, repeatability and practicability, and thus could be used in rat plasma lipid metabolomics study.

19.
Article in Chinese | WPRIM | ID: wpr-272686

ABSTRACT

To investigate the cause of liver toxicity induced by Polygoni Multiflori Radix through determining various mycotoxins in it. An UPLC-ESI-MS/MS method was developed and established to simultaneously determine 12 mycotoxins, Aflatoxins B₁, B₂, G₁, G₂, Ochratoxins A and B, Fumonisins B₁ and B₂,T-2 toxin, HT-2 toxin, Deoxynivalenol and Zearalenone, in rawand processed Polygon iMultiflori Radix. The sample was extracted with modified QuEChERS method, and then was separatedon a WelchUltimate XBC₁₈ column by gradient elution using methanol and 2 mmol•L⁻¹ ammonium acetate aqueous solution containing 0.1% acetic acidas mobile phase. The analytes were detected in MRM mode by mass spectrometry and determined by external standard method. This method made a good linearity in the 0.1-200 μg•kg⁻¹ with correlation coefficients of 0.996 3-0.999 9. The average recoveries of 12 mycotoxins at three spiked concentration levels were ranged from 71.19% to 98.68% with relative standard deviations of 1.7%-13%. This method is simple, sensitive, accurate and suitable for the quantification of 12 mycotoxins in Polygoni Multiflori Radix.As a result, 15 batches were found fungus contamination and total 8 kinds of mycotoxins including AFB₁, AFG₂, FB₁, OTB, T-2, HT-2, FB2 and OTA were detected, and their contentswere between 0.51-1 643.2 μg•kg⁻¹. Among these contaminated samples, AFB1 was detected in one batch of processed Polygoni Multiflori Radix with the content of 6.8 μg•kg⁻¹ beyond its limit standard 5 μg•kg⁻¹. Since AFB₁ has clear liver toxicity, we deduced that the mouldy samples may be one of the important causes of Polygoni Multiflori Radix causing liver toxicity.

20.
Article in Chinese | WPRIM | ID: wpr-275188

ABSTRACT

This paper aims to investigate the correlation between the antioxidant activity of Prunella vulgaris and its total phenolic acids content by measuring the antioxidant activity of different sources and different organs of P. vulgaris and the total contents of protocatechuic acid, protocatechuic aldehyde, caffeic acid, salviaflaside and rosmarinic acid in these samples. Using the 50% methanol extract of P. vulgaris samples as the research object, DPPH method and HPLC method were used respectively to determine the antioxidant activities and the total contents of the above-mentioned five analytes in P. vulgaris samples. 0.5 mL of 50% methanol extract of P. vulgaris reacts with 0.1 mmol•L⁻¹ DPPH ethanol solution for 60 min, then the absorbance of the reaction solution was measured at 517 nm, scavenging rate and IC₅₀ values were calculated by the absorbance and the sample concentration for evaluating the antioxidant activity. HPLC analysis was made on a C₁₈ Epic column, with acetonitrile-0.1% formic acid aqueous solution as mobile phase (gradient elution), and the detection wavelength was set at 280 nm. The correlation between the antioxidant capacity of different habitats and different organs of P. vulgaris and the total contents of five kinds of phenolic acids was analyzed by partial least squares method. The reaction dose-response range of 50% methanol extract of P. vulgaris with 0.1 mmol•L⁻¹ DPPH ethanol solution was 0.300-1.65 g•L⁻¹. When the quantities of potocatechuic acid, protocatechuic aldehyde, caffeic acid, salviaflaside and rosmarinic acid were respectively in 0.007 84-0.980, 0.011 5-1.44, 0.008 64-1.08, 0.080 0-1.00 and 0.079 8-0.998 μg range, their quantities were in good linear relationship with the corresponding peak areas. The average recovery of 5 components were 97.76%, 96.88%, 100.3%, 102.1%, 104.5%, with RSD of 1.8%, 1.6%, 1.7%, 1.6% and 1.7%, respectively. In a certain range of crude drug quantity, the antioxidant activity of each organ of P. vulgaris and total phenolic acids content inside has a good linear correlation. Therefore, in certain quality range of crude drug, DPPH bioassay combined with HPLC content determination can be used for the quality control of P. vulgaris, as is a new method for the quality control of P. vulgaris.

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