Method For Determination Of Content Research Articles

Quality control of Tianwang Buxin Pills based on UPLC fingerprint and multi-component quantification

Tianwang Buxin Pills have demonstrated therapeutic effects in clinical practice, whereas there is a serious lack of comprehensive quality control to ensure the safety and effectiveness of clinical medication. In this study, ultra-performance liquid chromatography(UPLC) was employed to establish the fingerprint and the method for simultaneously determining the content of seven components of Tianwang Buxin Pills. Furthermore, chemometrics was employed to identify the key factors for the stable quality, which provided a reference for the comprehensive quality control and evaluation of this preparation. There were 25 common peaks in the UPLC fingerprints of 15 batches of Tianwang Buxin Pills, from which thirteen compounds were identified. A quantitation method was established for seven pharmacological components(α-linolenic acid, salvianolic acid B, glycyrrhetinic acid, schisandrin A, β-asarone, 3,6'-disinapoylsucrose, and ligustilide). The principal component analysis(PCA) and partial least square discriminate analysis(PLS-DA) were performed to determine the key pharmacological components for controlling the quality stability of Tianwang Buxin Pills, which included 3,6'-disinapoylsucrose, α-linolenic acid, and β-asarone. The established fingerprint and multi-component content determination method have strong specificity, stability, and reliability. In addition, 3,6'-disinapoylsucrose, α-linolenic acid, and β-asarone are the key pharmacological components that ensure the quality stability between batches and can be used to comprehensively control the quality of Tianwang Buxin Pills. The findings provide a scientific basis for the quality evaluation and standard establishment of Tianwang Buxin Pills.

Solvents in the industrial synthesis of naphazoline nitrate: implementation of the principles of "Green chemistry" and analysis

The aim: implementation of the principles of green chemistry by regenerating the synthesis solvent 1,2,4-trichlorobenzene and reusing it during the synthesis of the Naphazoline nitrate substance. Study of the influence of the regenerated solvent on the quality of the final product by controlling analytical quality parameters. Development of a method for the quantitative determination and validation of synthesis solvents in a substance. Materials and methods: samples of the substance were synthesized according to the optimized proprietary technology of Farmak JSC. The obtained batches of fresh and regenerated 1,2,4-trichlorobenzene were analyzed according to the monograph of the European Pharmacopoeia on Naphazoline nitrate 0147. Results: the possibility of using regenerated 1,2,4-trichlorobenzene for the synthesis of the substance Naphazoline nitrate has been proven. It is shown that the regenerated solvent does not have a negative effect on the profile of impurities and the polymorphic form of the substance. Analytical quality parameters met the requirements of the internal specification and the requirements of the European Pharmacopoeia monograph. The developed and validated method of quantitative determination of synthesis solvents makes it possible to determine them at the required level. Conclusions: the introduction of regenerated 1,2,4-trichlorobenzene into the synthesis scheme made it possible to significantly reduce the amount of waste per 1 kg of product, which in turn significantly reduced the negative impact on the environment. Analytical quality parameters for regenerated 1,2,4-trichlorobenzene meet the requirements of the internal specification. Industrial series obtained on the regenerated solvent meet the requirements of the monograph of the European Pharmacopoeia. The polymorphic form of the substance batches manufactured on regenerated 1,2,4-trichlorobenzene corresponds to the polymorphic form of the substance batches manufactured on the fresh solvent. The obtained results on the influence of the regenerated solvent on the profile of impurities in the finished substance show the similarity of the profile of the series manufactured on both solvents. According to the requirements of ICH Q3C Impurities: Guideline for residual solvents, a method for quantitative determination of the residual content of 1,2,4-trichlorobenzene in the final product by gas chromatography was developed and validated. The absence of synthesis solvents at the limit of detection is shown

A comprehensive strategy for quality evaluation of Changan powder by fingerprinting combined with rapid qualitative and quantitative multi-ingredients profiling.

Changan powder (CAP) is mainly used to treat various intestinal diseases. Few studies on CAP have been reported; therefore, it is necessary to clarify the material basis of CAP to lay the foundation for further elucidating its functional mechanism and support the rational use of drugs. In the present study, we aimed to propose a methodology for the quality control of CAP based on qualitative and quantitative analysis of its components. An ultra-performance liquid chromatography coupled with Fourier transform ion cyclotron resonance mass spectrometry (UPLC-FT-ICR-MS) method was developed to identify chemical components in CAP. In addition, fingerprints of 10 different batches of CAP were established, and quantitative analysis based on UPLC was performed to analyze the quality of CAP. A total of 58 compounds were preliminarily characterized. The similarity of 10 batches of CAP was greater than 0.995, and 23 common peaks were calibrated. Investigation of the quantitative analytical methodology showed that the four components had good linear relationships within their respective concentration ranges (r2 ≥ 0.9992), and the relative standard deviation (RSD) of precision and stability was less than 2%. The RSD of sample recovery ranged from 0.78% to 1.52%. The established method can quickly and effectively identify the chemical components of CAP and accurately quantify the known components in CAP. The established fingerprinting and content determination method is stable, reliable, and easy to operate and can be applied in quality control and in vivo research on CAP.

Development and validation of an UHPLC-DAD method for oleandrin content determination in dried leaves of Nerium oleander from Eastern Algeria

This study aimed to develop and validate an UHPLC-DAD method for quantifying oleandrin in dried leaves and assessing its concentrations in samples from Eastern Algeria.For this purpose, a total of 100 leaf samples were collected from wild and cultivated shrubs across five provinces in Eastern Algeria during the flowering period. The UHPLC-DAD system was used to identify and quantify oleandrin. Chromatographic separation was performed using a Kinetex C18 Polar column (100 x 2.1 mm, 2.6 μm) from Phenomenex®. The flow rate was of 0.6 mL/min, and the detection wavelength was set at 220 nm.The mean oleandrin amount in dried leaf samples collected from the entire region was found to be 0.12 ± 0.12 mg/g. The analysis revealed statistically significant differences among the provinces and between wild and cultivated plants. These differences highlight potential disparities in the risk of acute poisoning in case of ingestion. However, no significant differences were observed among plants with different flower colors. Furthermore, no correlation was observed between the mean oleandrin levels and the meteorological parameters recorded during the annual survey of the harvest year, including temperature, humidity, sunshine, and cumulative rainfall. There was also no correlation between the mean, median, and 90th percentile oleandrin levels and the elevation of the collection sites.

Precise evaluation of batch adsorption kinetics of plant total polyphenols based on a flow-injection online spectrophotometric method.

Efficient evaluation of adsorption kinetics of plant total polyphenols is essential for the design of adsorption separation of bioactive compounds. The conventional method uses manual sampling with poor reproducibility. Here, we developed a new method for on-line determination of total polyphenol content (TPC) in plant extracts by applying the Folin-Ciocalteu method in flow-injection analysis (FIA). The FIA parameters were optimized and a standard curve with excellent linearity was established. Precise determination of TPC with a satisfactory sample throughput of 20 h-1 was achieved for the adsorption kinetic study. The pseudo-second-order kinetic model was found to better describe the kinetic parameters of the batch adsorption/desorption process. The developed method proved to be accurate compared with the conventional method. The FIA method holds significant promise for studying and monitoring adsorption processes, due to its automatic on-line nature, low consumption of reagents and samples, and the ability to generate large quantities of highly accurate adsorption data.

Screening of bioactive components endowing hawthorn with turbidity-eliminating and lipid-lowering functions and development of quality control method of hawthorn

Hawthorn has the efficacy of eliminating turbidity and lowering the blood lipid level, and it is used for treating hyperlipidemia in clinic. However, the bioactive components of hawthorn are still unclear. In this study, the spectrum-effect relationship was employed to screen the bioactive components of hawthorn in the treatment of hyperlipidemia, and then the bioactive components screened out were verified in vivo. Furthermore, the quality control method for hawthorn was developed based on liquid chromatography-mass spectrometry(LC-MS). The hyperlipidemia model of rats was built, and different polar fractions of hawthorn extracts and their combinations were administrated by gavage. The effects of different hawthorn extract fractions on the total cholesterol(TC), triglycerides(TG), and low-density lipoprotein-cholesterol(LDL-C) in the serum of model rats were studied. The orthogonal projections to latent structures(OPLS) algorithm was used to establish the spectrum-effect relationship model between the 24 chemical components of hawthorn and the pharmacodynamic indexes, and the bioactive components were screened out and verified in vivo. Finally, 10 chemical components of hawthorn, including citric acid and quinic acid, were selected to establish the method for evaluating hawthorn quality based on LC-MS. The results showed that different polar fractions of hawthorn extracts and their combinations regulated the TG, TC, and LDL-C levels in the serum of the model rats. The bioactive components of hawthorn screened by the OPLS model were vitexin-4″-O-glucoside, vitexin-2″-O-rhamnoside, rutin, citric acid, malic acid, and quinic acid. The 10 chemical components of hawthorn, i.e., citric acid, quinic acid, rutin, gallic acid, vitexin-4″-O-glucoside, vitexin-2″-O-rhamnoside, malic acid, vanillic acid, neochlorogenic acid, and fumaric acid were determined, with the average content of 38, 11, 0.018, 0.009 5, 0.037, 0.017, 8.1, 0.009 5, 0.073, and 0.98 mg·g~(-1), respectively. This study provided a scientific basis for elucidating the material basis of hawthorn in treating hyperlipidemia and developed a content determination method for evaluating the quality of hawthorn.

Quality evaluation of salt-fired Eucommiae Cortex based on HPLC fingerprint, multi-component content determination, and chemometrics

This study established an HPLC fingerprint and multi-component content determination method for salt-fired Eucommiae Cortex, and evaluated the quality of salt-fired Eucommiae Cortex from different sources using fingerprint similarity evaluation, cluster analysis(CA), principal component analysis(PCA), and orthogonal partial least square discriminate analysis(OPLS-DA). HPLC was launched on a Cosmosil 5C_(18)-MS-Ⅱ column(4.6 mm×250 mm, 5 μm) by gradient elution with a mobile phase of methanol-0.2% phosphoric acid aqueous solution at a flow rate of 1.0 mL·min~(-1), detection wavelength of 238 nm, column temperature of 30 ℃, and an injection volume of 10 μL. The results of fingerprint similarity evaluation for 20 batches of salt-fired Eucommiae Cortex indicated that, except for batch S3 with a similarity of 0.893, the similarity of the other 19 batches was of ≥ 0.919, suggesting good similarity. Fourteen common peaks were calibrated and seven common peaks were identified including geniposidic acid. The mass fractions of geniposidic acid, chlorogenic acid, geniposide, genipin, pinoresinol diglucoside, liriodendrin, and pinoresinol-4-O-β-D-glucopyranoside were 0.062 0%-0.426 9%, 0.024 9%-0.116 5%, 0.009 5%-0.052 9%, 0.005 5%-0.034 8%, 0.115 9%-0.317 8%, 0.016 4%-0.108 8%, and 0.026 4%-0.039 8%, respectively. Using CA, PCA, and OPLS-DA, the 20 batches of salt-fired Eucommiae Cortex were classified into three categories. Additionally, through the analysis of variable importance in projection(VIP) under OPLS-DA, two differential quality markers, geniposidic acid and chlorogenic acid, were identified. The established HPLC fingerprint and multi-component content determination method is stable and reliable, providing a reference for quality control of salt-fired Eucommiae Cortex.

Screening for Q-markers of Antiviral Granules based on neuraminidase inhibitors and Effect-constituent index

BackgroundAntiviral granules (AG) is a classic traditional Chinese medicine commonly employed for influenza treatment. However, there is an urgent need to improve its quality control standards. PurposeThe quality markers (Q-markers), guided by the Effect-constituent Index (ECI), were screened through in vitro and in vivo component identification, molecular docking, and neuraminidase (NA) inhibition experiments. MethodsThe chemical components in AG underwent analysis using UPLC-Q-Orbitrap HRMS and GC–MS, and serum pharmacochemistry was employed to analyze the components absorbed into the bloodstream. Molecular docking was used to evaluate the affinity of the prototype components to NA, and the inhibitory activity of the candidate components was later confirmed through NA inhibitor experiments. Following this, a UHPLC-MS/MS method was developed to screen and quantify the Q-markers in 20 sample batches. Lastly, the ECI was formulated using a multi-index comprehensive evaluation method that combines composition, content, and activity. ResultsA total of 246 compounds were identified in AG, and 89 prototype components and 19 metabolic components were detected in the serum of the rats. Molecular docking revealed that the binding energy of 35 candidate active ingredients was better than that of the original ligand and the target protein. Among these candidate active ingredients, 12 candidate Q-markers demonstrated significant inhibitory effects in NA inhibition experiments, with IC50 values ranging from 0.954 to 3.408 mM. A UHPLC-MS/MS content determination method was established for the quantification of 11 Q-markers, including Forsythiaside A, Pogostone, Verbascoside, Mangiferin, 5-methoxy-8-hydroxypsoralen, Curcumenol, Luteolin-7-glucuronide, Kaempferol-3-O-rutinoside, Baicalin, Rutin, and Bergaptol, in 20 batches of samples. The ECI was calculated based on activity and content of these Q-markers. Pearson's correlation analysis of the NA inhibitory effect of the samples and the ECI resulted in an R value of 0.859, indicating a good correlation. Furthermore, this correlation coefficient surpassed those observed between the content of each Q-marker and the NA inhibitory effect. ConclusionThe Q-markers for treating influenza with AG have been successfully screened, and the ECI of AG has been constructed. These findings will provide beneficial strategies for improving the quality control level of AG.

Quality by design tool evaluated green stability-indicating UPLC content determination method for the Olanzapine and Samidorphan dosage form

A green, environmentally friendly, quick, sensitive, cost-effective, stability-indicating, and analyst-friendly UPLC method for determining the content of Olanzapine and Samidorphan tablets formulation was developed since no method was reported in published articles. Waters CHS (50 × 2.1) mm, 1.7 um column, flow rate of 0.3 mL/min, injection volume of 1.0 µL, column temperature of 30 °C, detection wavelength of 232 nm, and a total runtime of 2 min were used to quantify the analytes. The mobile phase was composed of a solution containing 0.01 % di sodium phosphate and acetonitrile in the ratio of (30:70, v/v). The optimised technique has been validated, and the results are met the regulatory criteria. Olanzapine's accuracy results found from 99.5 % to 99.8 %, whereas Samidorphan accuracy results found from 99.4 % to 100.4 %. Olanzapine's precision and intermediate precision %RSD results found from 0.3 % to 0.7 %, whereas Samidorphan found from 0.5 % to 0.7 %. The correlation coefficient value for both analytes was found to be greater than 0.999 for the linearity range from 2.5 µg/mL to 15.0 µg/mL. Solution stability established for 24 hrs and filter compatibility studied. By studying forced degradation, the method stability indicating nature is proven. The method's robustness was assessed by utilising a design expert software tool. The method greenness was evaluated by using National method environmental index (NEMI), Green analytical procedure index (GAPI), Analytical greenness (AGREE) tools and Analytical Eco-Scale. AGREE value found 0.66 and eco-scale value found 81.

Harmonizing international quality standards for Andrographis paniculata: A comparative analysis of content determination methods across pharmacopeias

The quality standards for Andrographis paniculata, a widely used medicinal herb, exhibited significant variations across different pharmacopeias. In this study, we compared the HPLC content determination methods and total lactone content of A. paniculata samples from different regions, as specified in the Chinese (CP), United States (USP), European (EP), Thai (TP), and Indian pharmacopeias (IP), as well as the Hong Kong Chinese Materia Medica Standards (HK). We aimed to assess the differences and similarities among these pharmacopeias and harmonized international quality standards for A. paniculata. The analysis revealed variations in sample preparation, liquid chromatographic conditions, fingerprint profiles, and total lactone content among the different pharmacopeias. Specifically, the CP and HK methods exhibited superior sample preparation and chromatographic separation. Further comparing the content of 20 A. paniculata samples with the CP, USP, EP and HK methods showed consistent determinations for the same components, indicating similar detection capabilities. The discrepancies in total lactone content primarily stemmed from differences in the number and types of detected compounds. Moreover, the acceptance criteria exhibited a stringency in the order CP > HK > EP > USP. In conclusion, this comparison analysis of content determination in CP, USP, HK, EP, TP and IP provided a scientific foundation for the international standardization and trade regulations of A. paniculata. It also served as a valuable reference for the development of international quality standards for other medicinal herbs, facilitating the harmonization of global pharmaceutical standards.

Using the SWAT model to characterise the water regime of soils in agrolandscapes

The classification of soils water regimes a basic scientific basis in the form of an interdependent relationship between the movement of water and the formation of a soil profile, i. e. it is soil-genetic classification. This kind of classification provides a scientific and methodological platform for studying both the water regimes of soils in the landscape and the distribution of soils in the soil cover of the landscape. Numerical methods for representing the hydrological regimes of soils in the agricultural landscape are based on physically validated mathematical models of the soil water movement and spatial GIS information, which together allow to calculate, analyze and predict soil water regime, runoff in the scale of watersheds, substance transport in the soil profile, leaching processes, as well as the content of available soil moisture reserves in the agrolandscape structure – which is important for practice. A spatial-dynamic SWAT (Soil-Water-Atmosphere-Tool) model is presented to describe the water regimes of soils in the agro-landscape of the finite moraine ridge of the Upper Volga postglacial region (East European Plain, Tver region), as an example of landscape numerical hydrological models. Some examples are given in the article, which demonstrate that modeled data correspond well with experimental data on soil moisture dynamics in several points of agrolandscape for 3 depth levels, reflecting surface, deep (at groundwater level) and middle layers of soil profile, i. e. 10–20, 50–60 and 90–100 cm. On the one hand, the data were obtained by calculations with the help of the considered landscape-dynamic model; and on the other hand, – by classical soil drilling, sampling and gravimetric method for soil moisture content determination. It has been shown that the landscape model, adapted for specific conditions, using a digital elevation model with a resolution of 1×1 m per pixel, to calculate the soil water regime at different points of the agrolandscape satisfactorily describes the spatial-dynamic profile data on soil moisture.

Hepatoprotective activity of Patrinia scabiosaefolia Fisch and quality evaluation based on UPLC fingerprint and multi-component analysis

To establish a quality evaluation method for Patrinia scabiosaefolia Fisch (PS), as well as to study the anti-inflammatory and hepatoprotective effects of the aqueous extract of Patrinia scabiosaefolia Fisch (APS). We used ultra performance liquid chromatography (UPLC) to establish fingerprint and content determination method for PS. The alcoholic liver injury model was prepared by feeding Lieber-DeCarli alcohol liquid feed to mice. We determined the levels of ALT, AST, TC, TG in serum, as well as GSH, MDA in the liver. The mRNA relative expression levels of TNF-α, IL-6, IL-1β, INOS and COX-2 were detected by qRT-PCR, and liver tissues were taken for pathological examination. The fingerprints of 16 batches of PS were established, and 3 component peaks were identified, which were chlorogenic acid (CA), isochlorogenic acid A (ICAA) and isochlorogenic acid C (ICAC). The similarity of the 6 common peaks was between 0.924 and 1.000. A mice model of alcoholic liver injury was successfully made by mixing alcohol liquid feed. The levels of ALT, AST, TC and TG in serum and MDA, TNF-α, IL-1β, LL-6, COX-2 and INOS mRNA in liver were effectively reduced in the drug administration group. The levels of GSH in mouse liver tissue were increased in the drug administration group. The method has good repeatability, stability and feasibility, and it meets the requirements for Quality evaluation. APS exhibits a protective effect against alcoholic liver injury (ALI) in mice.

Comparison between two gypsum content determination methods applied to the study of soils in arid regions

With the scarcity, degradation of soils, the growing populations and the need to guarantee their food security, the valorization of gypsum soils widespread in arid and semi-arid regions is becoming a necessity. North African countries have a large part of their land area located in arid regions. It is therefore important to characterize the gypsum content using simple, rapid, economical and, environmentally friendly methods. Several methods have been proposed in the literature (chemical, thermogravimetric, and x-ray techniques). In this work, a comparison between two methods for gypsum determination in soils was undertaken. The first method of Coutinet is chemical and based on the use of BaSO4 for the precipitation of sulfate ions. The second method is Artieda method which is based on measuring the weight difference caused by the loss of crystalline water from gypsum molecules between the temperatures of 70 and 90 °C. To achieve the objective of this work, forty-three soil samples were analyzed. They were taken from two arid regions (Ouargla and Touggourt) located in the northern Sahara (Algeria). The soils contain gypsum accumulations. The results showed that most of the samples are slightly gypsiferous, with 36 and 32 samples for the Coutinet and Artieda methods respectively. A strong positive correlation (R2 = 0.95) exists between the results of the two methods studied. For gypsum contents higher than 2 %, the correlation coefficient is 0.94. However, for samples with contents less than 2 %, the correlation is very weak with R2=0.19. The Artieda method is thus encouraged for the gypsum quantification in soils of arid regions. This method is easy, requiring simple laboratory equipment (mainly a ventilated oven and a precision balance). Chemical methods have the disadvantage of being time-consuming and using expensive chemicals that are dangerous for the environment and human health.

Prediction and analysis of quality markers for Chuantieling gel patches based on HPLC fingerprinting and network pharmacology.

The Chuantieling gel patch (CGP), a traditional Chinese medicine compound, is an external treatment for asthma. It has shown remarkable effectiveness in alleviating asthma-related airway hyperresponsiveness and inflammation. Nevertheless, there is currently no information available regarding the analysis of quality markers for CGP, and there is a need for further improvement in quality control research. In this study, we developed an HPLC fingerprinting method for CGP and conducted a comprehensive methodological investigation. We assessed the similarity among 10 batches of CGP, identified common peaks, and quantified the content of seven major quality markers. Furthermore, we built a network pharmacology-based 'active ingredients-targets-pathways-diseases' network to forecast the potential mechanisms of action for the primary active components in asthma treatment. Our findings demonstrated that the developed CGP fingerprinting and content determination methods were consistent and trustworthy. We verified the existence of 25 shared peaks and successfully identified 7 chromatographic peaks, including sinigrin thiocyanate, ephedrine hydrochloride, methyleugenol, imperatorin, cinnamaldehyde, emodin, and 6-gingerol, using reference standards. The network pharmacology analysis suggested that these seven active components may target proteins such as STAT3 (signal transducer and activator of transcription 3), MAPK3 (mitogen-activated protein kinase 3), and TP53 (tumor protein P53) and influence various diseases through pathways including cancer pathways, hepatitis B, and PI3K-Akt (phosphoinositide 3-kinase-protein kinase B) signaling. This study provides insight into the complex multicomponent composition of CGP, and the predictive analysis through network pharmacology sets the stage for uncovering the mechanisms responsible for the therapeutic effects of CGP.

Degradation kinetics of β-nicotinamide mononucleotide based on reliable HPLC quantitative method

To explore the stability characteristics of β-nicotinamide mononucleotide(NMN) and provide data support for NMN production, preparation, and related product development, this study established a simple HPLC content determination method for NMN in simple substrate and investigated the degradation behavior, degradation products, and degradation kinetics of NMN under various chemical, physical, and biological conditions. The HPLC method employed a Welch Xtimate AQ-C_(18) column(4.6 mm×250 mm, 5 μm), a detection wavelength of 266 nm, a column temperature of 30 ℃, a flow rate of 1.0 mL·min~(-1), an injection volume of 5 μL, and a mobile phase consisting of methanol(A) and a 10 mmol·L~(-1) ammonium formate aqueous solution(B) with a gradient elution(0-6.7 min, 0-4% A; 6.7-13 min, 4%-18% A; 13-14.2 min, 18% A; 14.2-15 min, 18%-0 A; 15-22 min, 0 A). This method provided good separation between NMN and potential impurities and degradation products, and had a wide linear range, short analysis time, good durability, high accuracy, an average sample recovery rate of 98.71%, and an RSD of 1.2%. The instrument precision had an RSD of 0.26%, and the linearity within the examined range was excellent(R~2≥0.999 9). This method can be applied for NMN content determination in simple substrate. The degradation process of NMN in aqueous solution followed apparent first-order kinetics, with the degradation rate primarily influenced by high temperature and pH. NMN was more stable in low-temperature, neutral, or weakly acidic/alkaline environments. Strong acids or strong alkalis could accelerate its degradation, and its degradation rate was less affected by pepsin and trypsin. In an aqueous solution at room temperature, it followed the kinetic equation lg C_t=0.005 7t + 4.817 2, with t_(0.9) and t_(1/2) values of 95.58, 860.26 h, respectively. The results suggest that pH and temperature are the main factors affecting the stability of NMN in aqueous solution, and low temperature, moisture protection, and a weakly acidic environment are more conducive to the storage and application of NMN and its products.

Chemical Composition Analysis and Multi-index Component Content Determination of Compounds in Goupi Plaster Based on UPLC–Q-Exactive-MS and UPLC–MS/MS

ObjectiveThis study sought to evaluate and validate a method for chemical composition analysis and content determination of Goupi plaster components, a conventional prescription preparation of traditional Chinese medicine. This is geared toward providing a basis for quality control research and future development of Goupi plaster.MethodsUPLC–Q-Exactive-MS was used to qualitatively analyze the chemical components of Goupi plaster from different manufacturers in positive and negative ion modes. UPLC–MS/MS method was used to establish the determination methods for the detection of sinomenine, osthole, and cinnamaldehyde in Goupi plaster from different manufacturers.ResultsA total of 291 chemical components were identified in Goupi plaster from four manufacturers, including 97 chemical components with known source and pharmacological activity. Further, we determined the contents of sinomenine, osthole, and cinnamaldehyde.ConclusionIn summary, the UPLC–Q-Exactive-MS method was used to analyze the chemical components of Goupi plaster from different manufacturers. We established the UPLC–MS/MS method to determine the contents of sinomenine, osthole, and cinnamaldehyde in Goupi plaster from different manufacturers. The findings indicated that the method was comprehensive, rapid, and accurate, preliminarily revealing the material basis of Goupi plaster and providing a reference for follow-up development of Goupi plaster.

Study on the potential mechanism of Qingxin Lianzi Yin Decoction on renoprotection in db/db mice via network pharmacology and metabolomics

BackgroundDiabetic nephropathy (DN) was one of the most popular and most significant microvascular complications of diabetes mellitus. Qingxin Lianzi Yin Decoction (QXLZY) was a traditional Chinese classical formula, suitable for chronic urinary system diseases. QXLZY had good clinical efficacy in early DN, but the underlying molecular mechanism remained unrevealed. PurposeThis study aimed to establish the content determination method of QXLZY index components and explore the mechanism of QXLZY on DN by network pharmacology and metabolomics studies. MethodsFirstly, the content determination methods of QXLZY were established with calycosin-7-O-β-d-glucoside, acteoside, baicalin and glycyrrhizic acid as index components. Secondly, pharmacological experiments of QXLZY were evaluated using db/db mice. UHPLC-LTQ-Orbitrap MS was used to carry out untargeted urine metabolomics, serum metabolomics, and kidney metabolomics studies. Thirdly, employing network pharmacology, key components and targets were analyzed. Finally, targeted metabolomics studies were performed on the endogenous constituents in biological samples for validation based on untargeted metabolomics results. ResultsA method for the simultaneous determination of multiple index components in QXLZY was established, which passed the comprehensive methodological verification. It was simple, feasible, and scientific. The QXLZY treatment alleviated kidney injury of db/db mice, included the degree of histopathological damage and the level of urinary microalbumin/creatinine ratio. Untargeted metabolomics studies had identified metabolic dysfunction in pathways associated with amino acid metabolism in db/db mice. Treatment with QXLZY could reverse metabolite abnormalities and influence the pathways related to energy metabolism and amino acid metabolism. It had been found that pathways with a high degree were involved in signal transduction, prominently on amino acids metabolism and lipid metabolism, analyzed by network pharmacology. Disorders of amino acid metabolism did occur in db/db mice. QXLZY could revert the levels of metabolites, such as quinolinic acid, arginine, and asparagine. ConclusionThis study was the first time to demonstrate that QXLZY alleviated diabetes-induced pathological changes in the kidneys of db/db mice by correcting disturbances in amino acid metabolism. This work could provide a new experimental basis and theoretical guidance for the rational application of QXLZY on DN, exploring the new pharmacological effect of traditional Chinese medicine, and promoting in-depth research and development.

Fast and low-cost method for direct and simultaneous determination of nitrogen and carbon in soybean leaves using benchtop and portable near-infrared devices.

The current techniques for determining carbon and nitrogen content to provide information about the nutritional status of plants are time-consuming and expensive. For this reason, the objective of this study was to develop an analytical method for the direct and simultaneous determination of nitrogen and carbon elemental content in soybean leaves using near-infrared spectroscopy and compare the performance of conventional (1100-2500 nm spectral range) and portable equipment (1100-1700 nm spectral range). Partial least-squares regression models were developed using 27 soybean leaf samples collected during the 2021 harvest and applied for the simultaneous determination of carbon and nitrogen in 13 samples collected during the 2022 harvest. The root-mean-square error of prediction values for nitrogen and carbon were low (2.42 g kg-1 and 4.37 g kg-1 respectively) for the benchtop method yielded low but higher for the portable method (3.82 g kg-1 and 10.7 g kg-1 respectively). The benchtop method did not show significant differences when compared with the reference method for determining nitrogen and carbon. In contrast, the portable methodology showed potential as a screening method for determining nitrogen levels, particularly in fieldwork. The methodologies evaluated in this study were implemented and evaluated under real crop monitoring conditions, using independent sets of calibration and prediction samples. Their utilization enables the acquisition of cost-effective, safe analytical data aligning with the principles of green analytical chemistry. © 2023 Society of Chemical Industry.

Establishment of a quantitative method for GC analysis of polyoxyethylene (35) castor oil in microemulsion extracts

With the continuous exploration of microemulsions as solvents for traditional Chinese medicine extraction, polyoxyethy-lene(35) castor oil(CrEL), a commonly used surfactant, is being utilized by researchers. However, the problem of detecting residues of this surfactant in microemulsion extracts has greatly hampered the further development of microemulsion solvents. Based on the chemical structures of the components in CrEL and the content determination method of castor oil in the 2020 edition of the Chinese Pharmacopoeia(Vol. Ⅳ), this study employed gas chromatography(GC) and single-factor experiments to optimize the preparation method of methyl ricinoleate from CrEL. The conversion coefficient between the two was validated, and the optimal sample preparation method was used to process microemulsion extracts of Zexie Decoction from three batches. The content of methyl ricinoleate generated was determined, and the content of CrEL in the microemulsion extracts of Zexie Decoction was calculated using the above conversion coefficient. The results showed that the optimal preparation method for CrEL was determined. Specifically, 10 mL of 1 mol·L~(-1) KOH-methanol solution was heated at 60 ℃ for 15 min in a water bath. Subsequently, 10 mL of boron trifluoride etherate-methanol(1∶3) solution was heated at 60 ℃ for 15 min in a water bath, followed by extraction with n-hexane twice. CrEL could stably produce 20.84% methyl ricinoleate. According to this conversion coefficient, the average mass concentration of CrEL in the three batches of Zexie Decoction microemulsion extracts was 11.94 mg·mL~(-1), which was not significantly different from the CrEL mass concentration of 11.57 mg·mL~(-1) during microemulsion formulation, indicating that the established content determination method of this study was highly accurate, sensitive, and repeatable. It can be used for subsequent research on microemulsion extracts of Zexie Decoction and provide a reference for quality control of other drug formulations containing CrEL.

Determination of caffeine content in coffee drinks prepared in some coffee shops in the local market in Jeddah City, Saudi Arabia

Abstract The current study was aimed to develop a low cost HPLC method for determination of caffeine content in coffee samples in some coffee shops in Jeddah local market. Caffeine was extracted with water and separated through ZORBAX Eclipse XDB C-18 column using methanol/water (40:60) as mobile phase. The average peak response time for caffeine was 2.747 min with a relative standard deviation of 1.061. The proposed assay was able to detect caffeine in the concentration range from 5 to 45 ppm with limits of detection (LOD = 3σ/b) and quantification (LOQ = 10σ/b) of 1.086 and 3.619 ppm using two-channel UV detector set at 274 and 264 nm with correlation coefficient (R 2) of 0.9996, respectively. The assay was adopted for the determination caffeine content in 30 coffee samples collected from eight brand coffee shops and from local market. Each sample was injected in triplicate (n = 3) and the average and confidence limit of the mean were calculated. The concentration of caffeine in coffee brand shops varied from 513.82 ± \pm 12.91 to 8080.05 ± \pm 3.06 ppm, whereas in beans and instant coffee its content was diverse from 360.18 ± \pm 86.72 to 1306.98 ± \pm 27.31 ppm. These results were validated using Student’s t-test at 95% confidence level.