Ammonium bicarbonate buffers combined with hybrid surface technology columns improve the peak shape of strongly tailing lipids.

BACKGROUND: Lipids such as phosphatidic acids (PAs) and cardiolipins (CLs) present strongly tailing peaks in reversed phase liquid chromatography, which entails low detectability. They are usually analyzed by hydrophilic interaction liquid chromatography (HILIC), which hampers high-throughput lipidomics. Thus, there is a great need for improved analytical methods in order to obtain a broader coverage of the lipidome in a single chromatographic method. We investigated the effect of ammonium bicarbonate (ABC) on peak asymmetry and detectability, in comparison with ammonium formate (AFO) on both a conventional BEH C18 column and an HST-CSH C18 column. RESULTS: The combination of 2.5 mM ABC buffer pH 8 with an HST-CSH C18 column produced significantly improved results, reducing the asymmetry factor at 10 % peak height of PA 16:0/18:1 from 8.4 to 1.6. Furthermore, on average, there was up to a 54-fold enhancement in the peak height of its [M - H]- ion compared to AFO and the BEH C18 column. We confirmed this beneficial effect on other strongly tailing lipids, with accessible phosphate moieties e.g., cardiolipins, phosphatidylinositol phosphate, phosphatidylinositol bisphosphate, phosphorylated ceramide and phosphorylated sphingosine. Furthermore, we found an increased detectability of phospho- and sphingolipids up to 28 times in negative mode when using an HST-CSH C18 column. The method was successfully applied to mouse liver samples, where previously undetected endogenous phospholipids could be analyzed with improved chromatographic separation. SIGNIFICANCE: In conclusion, the use of 2.5 mM ABC substantially improved the peak shape of PAs and enhanced the detectability of the lipidome in negative mode on an RPLC-ESI-Q-TOF-MS system on both BEH C18 and HST-CSH C18 columns. This method provides a wider coverage of the lipidome with one single injection for future lipidomic applications in negative mode.

Discovery of quality markers of Phyllanthus emblica by integrating chromatographic fingerprint, serum pharmacochemistry and network pharmacology.

Phyllanthus emblica (P. emblica) is a vital medicinal plant with both medical and edible values. In the quality standard of P. emblica listed by the Chinese Pharmacopoeia, gallic acid is used as the index component for the content determination. However, a large number of tannin components can be decomposed into gallic acid during its refluxing extraction process, thus affecting the accuracy and specificity of the content determination. Thus, the index component used for the quality control needs to be further determined. In this study, the quality markers of P. emblica was specified by integrating chromatographic fingerprint, serum pharmacochemistry and network pharmacology. The chromatographic fingerprint of 18 batches of P. emblica samples were established by ultra-high-performance liquid chromatography (UPLC), and 8 differential components causing quality fluctuation were identified by chemometric analysis and UPLC-Q-TOF/MS analysis. Afterwards, 14 prototype migration components absorbed into the blood after gavage administration to rats were identified by UPLC-Q-TOF/MS analysis. Subsequently, a network pharmacology approach was used to construct the component-target-disease-pathway network, resulting in the identification of 22 components responsible for efficacy of P. emblica. Finally, by integrating the above results, ellagic acid was screened out as one of the Q-markers and could be employed as a quantitative component of P. emblica to improve the quality standard. The strategy is also informative for discovering Q-markers of other TCMs.

A Comprehensive Study for Determination of Free Fatty Acids in Selected Biological Materials: A Review.

The quality of oil is highly dependent on its free fatty acid (FFA) content, especially due to increased restrictions on renewable fuels. As a result, there has been a growing interest in free fatty acid determination methods over the last few decades. While various standard methods are currently available, such as the American Oil Chemists Society (AOCS), International Union of Pure and Applied Chemistry (IUPAC), and Japan Oil Chemists' Society (JOCS), to obtain accurate results, there is a pressing need to investigate a fast, accurate, feasible, and eco-friendly methodology for determining FFA in biological materials. This is owing to inadequate characteristics of the methods, such as solvent consumption and reproducibility, among others. This study aims to investigate FFA determination methods to identify suitable approaches and introduce a fresh perspective.

Chromatographic Methods and Sample Pretreatment Techniques for Aldehydes, Biogenic Amine, and Carboxylic Acids in Food Samples.

This review paper critically examines the current state of research concerning the analysis and derivatization of aldehyde, aromatic hydrocarbons and carboxylic acids components in foods and drinks samples, with a specific focus on the application of Chromatographic techniques. These diverse components, as vital contributors to the sensory attributes of food, necessitate accurate and sensitive analytical methods for their identification and quantification, which is crucial for ensuring food safety and compliance with regulatory standards. In this paper, High-Performance Liquid Chromatography (HPLC) and Gas Chromatographic (GC) methods for the separation, identification, and quantification of aldehydes in complex food matrices were reviewed. In addition, the review explores derivatization strategies employed to enhance the detectability and stability of aldehydes during chromatographic analysis. Derivatization methods, when applied judiciously, improve separation efficiency and increase detection sensitivity, thereby ensuring a more accurate and reliable quantification of aldehyde aromatic hydrocarbons and carboxylic acids species in food samples. Furthermore, methodological aspects encompassing sample preparation, chromatographic separation, and derivatization techniques are discussed. Validation was carried out in term of limit of detections are highlighted as crucial elements in achieving accurate quantification of compounds content. The discussion presented by emphasizing the significance of the combined HPLC and GC chromatography methods, along with derivatization strategies, in advancing the analytical capabilities within the realm of food science.

Characterization of reversed-phase liquid chromatographic columns containing positively charged functionality.

To date, the most commonly used column characterization databases do not determine the relative positive charge associated with new generation RP columns, or they fail to successfully discriminate between RP columns of purportedly low level positive and neutral characters. This paper rectifies this in that it describes a convenient and robust chromatographic procedure for the assessment of the low levels of positive charge on a range of RP columns. The low degree of positive charge was determined by their electrostatic attraction towards the negatively charged 4-n-octylbenzene sulfonic acid (4-OBSA) relative to their retention of the hydrophobic marker toluene (Tol). The new parameter (α4-OBSA/Tol) was determined for 15 commercially available RP-LC columns. When this was combined with existing Tanaka parameters it was possible to guide the chromatographer towards similar columns as "backup / equivalent phases" or dissimilar columns for exploitation in method development strategies. It should be noted that under certain chromatographic conditions the retention mechanism(s) may be too complex to allow direct location of a "backup / equivalent" column(s). The α4-OBSA/Tol results indicate that even the new generation neutral alkyl phases may exhibit a small degree of positive charge at low buffer concentrations. Mobile phases containing low % MeCN were demonstrated to promote mixed mode (anionic exchange / hydrophobic) retention whereas at high % MeCN anionic exchange retention dominated. The measure of electrostatic repulsion between positively charged columns and positively charged bases was assessed by evaluating the relative retention of a range of bases and neutral analytes. The greatest electrostatic repulsion was observed with hydrophilic bases. While there was no correlation between the positive charge associated with the phases assessed by electrostatic attraction or repulsion, the columns could be broadly divided into three subsets (i.e., significant positive character, medium to low positive character and insignificant positive character). Finally, the results were used to highlight the usefulness of the column characterization database containing the new anionic exchange retention parameter (α4-OBSA/Tol) for the selection of an equivalent column possessing a low level of positive character in the analysis of a real-life biopharmaceutical application.

[Preparation and application of chromatographic stationary phase based on two-dimensional materials].

The stationary phase is the heart of chromatographic separation technology and a critical contributor to the overall separation performance of a chromatographic separation technique. However, traditional silicon-based materials designed for this purpose usually feature complex preparation processes, suboptimal permeability, pronounced mass-transfer resistance, and limited pH-range compatibility. These limitations have spurred ongoing research efforts aimed at developing new chromatographic stationary phases characterized by higher separation efficiency, adaptable selectivity, and a broader scope of applicability. In this context, the scientific community has made significant strides toward the development of new-generation materials suitable for use as chromatographic stationary phases. These materials include carbon-based nanomaterial arrays, carbon quantum dots, and two-dimensional (2D) materials. 2D-materials are characterized by nanometer-scale thicknesses, extensive specific surface areas, distinctive layered structures, and outstanding mechanical properties under standard conditions. Thus, these materials demonstrate excellent utility in various applications, such as electrical and thermal conductivity enhancements, gas storage and separation solutions, membrane separation technologies, and catalysis. Graphene, which is arguably the most popular 2D-material used for chromatographic separation, consists of a 2D-lattice of carbon atoms arranged in a single layer, with a large specific surface area and efficient adsorption properties. Its widespread adoption in research and various industries is a testament to its versatility and effectiveness. In addition to graphene, the scientific community has developed various 2D-materials that mirror the layered structures of graphene, such as boron nitride, transition-metal sulfides, and 2D porous organic frameworks, all of which offer unique advantages. 2D porous organic frameworks, in particular, have received attention because of their nanosheet morphology, one-dimensional pores, and special interlayer forces; thus, these frameworks are considered promising candidate chromatographic stationary phase materials. Such recognition is especially true for 2D-metal organic frameworks (MOFs) and 2D-covalent organic frameworks (COFs), which exhibit low densities, high porosities, and substantial specific surface areas. The modifiability of these materials, in terms of pore size, shape, functional groups, and layer-stacking arrangements allows for excellent separation selectivity, highlighting their promising potential in chromatographic separation. Compared with their three-dimensional counterparts, 2D-MOFs feature a simple pore structure that offers reduced mass-transfer resistance and enhanced column efficiency. These attributes highlight the advantages of 2D-MOF nanosheets as chromatographic stationary phases. Similarly, 2D-COFs, given their high specific surface area and porosity, not only exhibit great thermal stability and chemical tolerance but also support a wide selection of solvents and operational conditions. Therefore, their role in the preparation of chromatographic stationary phases is considered highly promising. This review discusses the latest research developments in 2D porous organic framework materials in the context of gas- and liquid-chromatographic stationary phases. It introduces the synthesis methods for these novel materials, elucidates their retention mechanisms, and describes the applications of other 2D-materials, such as graphene, its derivatives, graphitic carbon nitride, and boron nitride, in chromatography. This review aims to shed light on the promising development prospects and future directions of 2D-materials in the field of chromatographic separation, offering valuable insights into the rational design and application of new 2D-materials in chromatography.

[Recent progress of chromatographic techniques for antibody purification].

Antibody drugs are becoming increasingly popular in disease diagnosis, targeted therapy, and immunoprevention owing to their characteristics of high targeting ability, strong specificity, low toxicity, and mild side effects. The demand for antibody drugs is steadily increasing, and their production scale is expanding. Upstream cell culture technology has been greatly improved by the high-capacity production of monoclonal antibodies. However, the downstream purification of antibodies presents a bottleneck in the production process. Moreover, the purification cost of antibodies is extremely high, accounting for approximately 50%-80% of the total cost of antibody production. Chromatographic technology, given its selectivity and high separation efficiency, is the main method for antibody purification. This process usually involves three stages: antibody capture, intermediate purification, and polishing. Different chromatographic techniques, such as affinity chromatography, ion-exchange chromatography, hydrophobic interaction chromatography, mixed-mode chromatography, and temperature-responsive chromatography, are used in each stage. Affinity chromatography, mainly protein A affinity chromatography, is applied for the selective capture and purification of antibodies from raw biofluids or harvested cell culture supernatants. Other chromatographic techniques, such as ion-exchange chromatography, hydrophobic interaction chromatography, and mixed-mode chromatography, are used for intermediate purification and antibody polishing. Affinity biomimetic chromatography and hydrophobic charge-induction chromatography can produce antibodies with purities comparable with those obtained through protein A chromatography, by employing artificial chemical/short peptide ligands with good selectivity, high stability, and low cost. Temperature-responsive chromatography is a promising technique for the separation and purification of antibodies. In this technique, antibody capture and elution is controlled by simply adjusting the column temperature, which greatly eliminates the risk of antibody aggregation and inactivation under acidic elution conditions. The combination of different chromatographic methods to improve separation selectivity and achieve effective elution under mild conditions is another useful strategy to enhance the yield and quality of antibodies. This review provides an overview of recent advances in the field of antibody purification using chromatography and discusses future developments in this technology.

Validated chromatographic approach for determination of two ternary mixtures in newly approved formulations for helicobacter pylori eradication: assessment of greenness profile and content uniformity.

A new, sensitive, and rapid isocratic reversed phase chromatographic method (RP-HPLC-UV) was developed for simultaneous separation of two newly co-formulated antiulcer mixtures; Amoxicillin, Vonoprazan and Clarithromycin [Mixture (I)], and Amoxicillin, Lansoprazole and Clarithromycin [Mixture (II)]. Analytical separation was performed using a Promosil C18 column and ultraviolet detection at 210 nm. The separation was achieved within only 8 min. For both mixtures, an aqueous solution, composed of (Acetonitrile: Methanol: 0. 2 M phosphoric acid) within ratio of (30: 30: 40) adjusted to final pH 3.0, was the mobile phase. This method was validated as per the International Conference on Harmonization guidelines. The linearity ranges of these proposed method of the (Mixture (I)) were 25.0-400.0 µg/mL Amoxicillin, 0.5-8.0 µg/mL Vonoprazan, and 12.5-200.0 µg/mL Clarithromycin. And the linearity ranges of the (Mixture (II)) were 10.0-300.0 µg/mL Amoxicillin, 0.3-9.0 µg/mL Lansoprazole and 5.0-150.0 µg/mL Clarithromycin. This method was firstly applied for effective separation of Amoxicillin, Vonoprazan and Clarithromycin [Mixture (I)]. It fulfilled good repeatability, sensitivity, and accuracy (R.S.D. < 2.0%). The mean recoveries of the analytes in their Tri-Pak formulations were acceptable. The greenness of the developed chromatographic methods was assessed using an Eco-scale method and it was applied for content uniformity testing as per the United States Pharmacopoeia (USP) and the acceptance value of Amoxicillin, in Mixture (I) was 2.88, the acceptance values for Amoxicillin, Lansoprazole in Mixture (II) were 2.592, 2.424, respectively.

A fungal hyphae-derived biomass carbon for magnetic solid-phase extraction of the organochlorine pesticides in water samples, tea beverages, and Chinese traditional medicines before gas chromatography-tandem mass spectrometry determination.

A magnetic biochar nanomaterial derived from fungal hyphae was introduced into the sample preparation field. The magnetic fungal hyphae-derived biomass carbon (MFHBC) could be produced by a controllable hydrothermal method. In order to obtain the best sorbent for magnetic solid-phase extraction (MSPE), the reaction conditions containing temperature, time and the consumption of fungal hyphae were investigated. A series of MFHBC materials were characterized by vibrating sample magnetometers, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and transmission electron microscopy. A material with a satisfactory saturation magnetization (21.58 emu g-1) and largest surface area (88.06 m2 g-1) was selected as the sorbent to extract ten typical organochlorine pesticides (OCPs). The extraction conditions were optimized as 20 mL of sample solution with 70 mg of sorbent and 2.0 g of NaCl oscillated at 50 °C for 5.0 min. And the optimum desorption was performed by oscillating sorbent in 1.0 mL acetonitrile for 5.0 min. Then, the MFHBC-based MSPE-GC-MS/MS methods were established for different samples including water samples, tea beverages, and Chinese traditional medicines. The linearities were 10-2500 ng L-1 or 100-25,000 ng kg-1, and the limits of detection were 0.3-13.9 ng L-1 for water sample, 0.1-9.7 ng L-1 for tea beverage samples, 0.1-21.4 ng L-1 for Shenqi Fuzheng injection samples, and 7.2-278.3 ng kg-1 for Astragali Radix decoction pieces. Except for satisfactory repeatability (RSDs ≤13.8%) in intra-day and inter-day tests (n = 3), the reproducibility (RSDs ≤13.5%, n = 3) of MFHBC was acceptable. The methods were applied in the determination of OCPs from above real samples, with the recoveries of 80.5-117.2% and the RSDs (n = 3) <8.9%. The methods were suitable in the sensitive determination of OCPs from simple to complex matrix samples.

Resin screening and process optimization for erythritol mother liquor chromatographic separation.

In order to improve the utilization value of the erythritol mother liquor, the separation and purification of the erythritol mother liquor was selected in this study. The selected chromatographic separation programme for erythritol crystallizing mother liquor is as follows: Firstly, erythritol is resolved from mannitol and arabitol with DTF-01Ca (Suqing Group) resin and then mannitol is resolved from arabitol with 99Ca/320 (Dowex) resin. At the same time, the chromatographic conditions of the DTF-01Ca (Suqing Group) and 99Ca/320 (Dowex) resins were optimized, resulting in an optimal separation temperature and mobile phase flow rate of 70 °C, 10 ml/min. On this basis, a single-column chromatographic model was used to calculate the TD model parameter (N) and the mass transfer coefficient (km ) of the separation of erythritol mother liquor by DTF-01Ca (Suqing Group) and 99Ca/320 (Dowex) resins. The adsorption isotherms, TD model parameter (N) and the mass transfer coefficient (km ) provides data references for the design and operation of the simulated moving beds (SMB) separation system for the industrial-scale separation of erythritol crystallizing mother liquor.

Chemometric-based drug discovery approaches from natural origins using hyphenated chromatographic techniques.

INTRODUCTION: Isolation and characterization of bioactive components from complex matrices of marine or terrestrial biological origins are the most challenging issues for natural product chemists. Biochemometric is a new potential scope in natural product analytical science, and it is a methodology to find the compound's correlation to their bioactivity with the help of hyphenated chromatographic techniques and chemometric tools. OBJECTIVES: The present review aims to evaluate the application of chemometric tools coupled to chromatographic techniques for drug discovery from natural resources. METHODS: The searching keywords "biochemometric," "chemometric," "chromatography," "natural products bioassay," and "bioassay" were selected to search the published articles between 2010-2023 using different search engines including "Pubmed", "Web of Science," "ScienceDirect," and "Google scholar." RESULTS: An initial stage in natural product analysis is applying the chromatographic hyphenated techniques in conjunction with biochemometric approaches. Among the applied chromatographic techniques, liquid chromatography (LC) techniques, have taken up more than half (53%) and also, mass spectroscopy (MS)-based chromatographic techniques such as LC-MS are the most widely used techniques applied in combination with chemometric methods for natural products bioassay. Considering the complexity of dataset achieved from chromatographic hyphenated techniques, chemometric tools have been increasingly employed for phytochemical studies in the context of determining botanicals geographical origin, quality control, and detection of bioactive compounds. CONCLUSION: Biochemometric application is expected to be further improved with advancing in data acquisition methods, new efficient preprocessing, model validation and variable selection methods which would guarantee that the applied model to have good prediction ability in compound relation to its bioactivity.

Development of a novel UPLC approach to co-prediction of four active compounds in a multi-component pharmaceutical preparation.

In this work, a new ultra-performance liquid chromatography method based on photodiode array detection (UPLC-PDA) was first developed for the quantitative analysis of the quaternary mixture of ascorbic acid (AA), paracetamol (PAR), caffeine (CAF) and chlorpheniramine maleate (CPA) in a commercial dosage form. The developed UPLC-PDA method offered a new possibility for the co-determination of four active ingredients in a drug combination with short run time and simple sample preparation. The successful chromatographic separation of the four drugs was performed using a Waters Acquity UPLC BEH C18 column (1.7 µm 2.1 × 100 mm) (Mildford, USA) and a mobile phase consisting of water (12 %), acetonitrile (13 %) and 0.1 M H3PO4 (75 %) at a flow rate of 0.25 mL/min. The validation of the proposed UPLC-PDA approach was verified by analyzing synthetic mixtures, inter- and intra-day experiments, and commercial powder samples and provided satisfactory results.

Changes in chemical properties and microbial communities' composition of a forest litter-based biofertilizer produced through aerated solid-state culture under different oxygen conditions.

Fermented forest litter (FFL) is a bioproduct used as biofertilizer for several decades in Eastern Asia and Latin America. It is locally handcrafted by farmers in anaerobic conditions by fermenting forest litter added with agricultural by-products such as whey, cereal bran, and molasses. The aim of this study was to characterize the FFL process and product through gas and liquid chromatography analyses. It also provides some highlights on the influence of O2 on this solid-state culture. Under anoxic condition, a maximum CO2 production rate (CDPR) of 0.41 mL/h∙g dry matter (dm) was reached after 8 days. The main volatile organic compounds (VOCs) were ethanol and ethyl acetate, with a production rate profile similar to CDPR. After 21 days of culture, no residual sucrose nor lactose was detected. Lactic and acetic acids reached 58.8 mg/g dm and 10.2 mg/g dm, respectively, ensuring the acidification of the matrix to a final pH of 4.72. A metabarcoding analysis revealed that heterolactic acid bacteria (Lentilactobacillus, Leuconostoc), homolactic acid bacteria (Lactococcus), and yeasts (Saccharomyces, Clavispora) were predominant. Predicted genes in the microbiome confirmed the potential link between detected bacteria and acids and VOCs produced. When O2 was fed to the cultures, final pH reached values up to 8.5. No significant amounts of lactic nor acetic acid were found. In addition, a strong shift in microbial communities was observed, with a predominance of Proteobacteria and molds, among which are potential pathogens like Fusarium species. This suggests that particular care must be brought to maintain anoxic conditions throughout the process.

Flavonoids isolated from Vismia macrophylla Kunth against resistant bacteria.

The antimicrobial activity of Vismia macrophylla extract is reported in the literature; however, little is known about the presence of phenolic compounds and their antimicrobial activity in this species. This study aimed to isolate phenolic compounds with antimicrobial action from the leaves of V. macrophylla. The ethanolic extract (VmL-Et) was submitted to sephadex column separation, and some fractions were submitted to derivatization with BSTFA and analysed by GC-MS. This study indicated the presence of the catechin, osajaxanthone, quercetin, quercitrin, and glucodistylin. Of these, osajaxanthone, quercetin, quercitrin, and glucodistylin were isolated and identified by spectroscopic techniques. VmL-Et, quercetin, quercitrin, glucodistylin, and maslinic acid, were tested against the Acinetobacter baumannii, Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Enterococcus faecalis. The results showed broad spectrum action of the extract Vm-Et, glucodistylin and quercitrin. The species V. macrophylla occurring in the Brazilian biome showed potential for obtaining phenolic compounds that can help combat microbial resistance.

A new chromatographic response function with automatically adapting weight factor for automated method development.

A critical factor for automated method development in chromatography is the maximization or minimization of an objective function describing the quality (and speed) of the separation. In chromatography, this function is commonly referred to as a chromatographic response function (CRF). Many CRFs have previously been introduced, but many have unfavourable properties such as featuring multiple optima, insufficient discriminatory power, and a too strong dependence on the weight factors needed to balance resolution and time penalty components. To overcome these problems, the present study introduces a new type of CRF wherein the relative weight of the time penalty term is a self-adaptive function of the separation quality. The ability to unambiguously identify the optimal gradient settings of this newly proposed CRF is compared to that of some of the most frequently used CRFs in a study covering 100 randomly composed in silico samples. Doing so, the new CRF is found to flawlessly lead to the correct solution (=linear gradient parameters providing the highest resolution in the shortest potential time) in 100 % of the cases, while the most frequently used literature CRFs were off-target for about 50 to 60 % of the samples, even when considering the availability of spectral peak shape data. Some slight alterations to the proposed CRF are introduced and discussed as well.

Green synthesis of N-rich carbon dot-derived crosslinked covalent organic nanomaterial for multipurpose chromatographic applications.

Carbon dots (CDs) derived crosslinked covalent organic nanomaterials (CONs) possessing high specific surface area and abundant surface functional groups are considered to be potential candidates for multimodal chromatographic separations. Typically, the synthesis of CDs and CONs requires harsh reaction conditions and toxic organic solvents, hence, the pursuit of facile and mild preparation strategies is the goal of researchers. In this work, 3-aminopropyltriethoxysilane and D-glucose were used as nitrogen and carbon sources, respectively, to prepare amino-CDs (AmCDs) by rapid low-temperature polymerization rather than the common high-temperature and high-pressure reaction. Then, surface functionalization of the aminated silica gel was carried out in a deep eutectic solvent by using hydrophilic AmCDs and 1,3,5-triformylbenzene (TFB) as the functional monomers. Consequently, a novel N-rich CDs derived CON surface-functionalized silica gel (AmCDs-CON@SiO2) was obtained under mild reaction conditions. The combination of AmCDs and TFB created an ideal CON based chromatographic stationary phase. The incorporation of TFB not only contributed to the successful construction of a crosslinked CON, but also enhanced the interaction forces. The developed AmCDs-CON@SiO2 has a great potential for versatile applications in liquid chromatography. This study proposes a simple stationary phase preparation strategy by the surface modification of silica gel with CDs-based CON. Moreover, this study verified the application potential of CDs derived CON in chromatographic separation. This not only promotes the development of CDs in the field of liquid chromatographic stationary phase, but also provides some reference value for the wide application of cross-linked CON.

Transformer fault diagnosis based on adversarial generative networks and deep stacked autoencoder.

Establishing a deep learning model for transformer fault diagnosis using transformer oil chromatogram data requires a large number of fault samples. The lack and imbalance of oil chromatogram data can lead to overfitting, lack of representativeness of the model, and unsatisfactory prediction results on test set data, making it difficult to accurately diagnose transformer faults. A conditional Wasserstein generative adversarial network with gradient penalty optimization (CWGAN-GP) is adopted in this paper, which based on gradient penalty optimization and expand the oil chromatography fault samples of 500 sets of transformer oil chromatography data with 5 types of faults. The proposed method is used to classify transformer faults using a deep autoencoder, and the sample quality of the neural network model proposed in this paper is compared with several other variants of generative adversarial neural network models. The research results show that after using the method proposed in this paper for sample expansion, the overall accuracy of fault diagnosis can reach 93.2 %, which is 4.98 % higher than the original imbalanced samples. Compared with other sample expansion methods, the accuracy of fault diagnosis of the algorithm in this paper is improved by 1.70 %-3.05 %.

Thorough Validation of Optimized Size Exclusion Chromatography-Total Organic Carbon Analysis for Natural Organic Matter in Fresh Waters.

Size exclusion chromatography with total organic carbon detection (HPSEC-TOC) is a widely employed technique for characterizing aquatic natural organic matter (NOM) into high, medium, and low molecular weight fractions. This study validates the suitability of HPSEC-TOC for a simplified yet efficient routine analysis of freshwater and its application within drinking water treatment plants. The investigation highlights key procedural considerations for optimal results and shows the importance of sample preservation by refrigeration with a maximum storage duration of two weeks. Prior to analysis, the removal of inorganic carbon is essential, which is achieved without altering the NOM composition through sample acidification to pH 6 and subsequent N2-purging. The chromatographic separation employs a preparative TSK HW-50S column to achieve a limit of detection of 19.0 µgC dm-3 with an injection volume of 1350 mm-3. The method demonstrates linearity up to 10,000 µgC dm-3. Precision, trueness and recovery assessments are conducted using certified reference materials, model compounds, and real water samples. The relative measurement uncertainty in routine analysis ranges from 3.22% to 5.17%, while the measurement uncertainty on the bias is 8.73%. Overall, the HPSEC-TOC represents a reliable tool for NOM fractions analysis in both treated and untreated ground and surface water.

[Transformation of scientific research results into teaching resources to improve the teaching effect: taking the teaching of the chromatographic method in the pharmaceutical analysis course as an example].

The pharmaceutical analysis course is a three-dimensional knowledge network that connects several courses to form a new comprehensive knowledge node involving a large knowledge system and flexible knowledge structure. In this course, the subject of chromatography covers a wide range of topics. However, because accurate content is challenging to present, the teaching effect of this subject is poor. In this work, we sought to achieve the educational purpose of establishing morality and cultivating talent, as well as the goal of training highly skilled professionals, by taking the teaching of chromatography in the pharmaceutical analysis course as an example of transforming scientific research results into teaching resources. The resources obtained are integrated into the teaching process to provide innovative and scientific research ideas to students with the aim of not only helping them understand and master technical knowledge but also exercise their ability to raise and solve problems. Furthermore, we expound on how to introduce scientific development frontiers and formulate scientific problems through curriculum design. We also describe how our strategy can promote the teaching effect and achieve teaching objectives. Based on the characteristics of rapid knowledge update and equal emphasis on theory and practice in pharmaceutical analysis, the course is designed by introducing new advances in scientific development, formulating scientific problems, and adopting question- and problem-based learning methods for teaching. The teaching effect is then evaluated through diversified assessment, student feedback, and self-evaluation. The results show that the transformation of scientific research results into teaching resources plays a significant role in stimulating students' interest in learning, improving students' ability to solve problems, and achieving curriculum objectives, all of which greatly improve the teaching effect.

Purity control of simulated moving bed based on advanced fuzzy controller.

Simulated moving bed (SMB) technology is considered one of the most successful techniques in chromatographic separation. However, due to the nonlinearity caused by discrete events and sensitivity to numerous separation performance parameters, purity control in SMB systems has been a challenging issue. Fuzzy controllers are increasingly popular in industrial environments due to their simplicity and effectiveness in handling nonlinearity. However, traditional fuzzy controllers used in industry often overlook considerations of error acceleration, resulting in slight deviations from target values under steady-state conditions and oscillatory behavior when system parameters change. This study proposes an advanced fuzzy controller, where in a series of experiments, the purity control targets for component B are set at 94% and 96%, and for component A are set at 96% and 96%, respectively. Experimental results indicate that the advanced fuzzy controller achieves higher precision, with an average deviation of around 0.1%, for both components B and A. Importantly, under variations in adsorbent parameter(from 0.01 to 0.03), feed concentration(from 4.5 to 5.2), and switching time(from 178 to 182), the experimental results demonstrate smoother control with the advanced controller, particularly when oscillations occur with conventional fuzzy controllers due to switching time variations, indicating robust control with the advanced fuzzy controller.