Simple and sensitive determination of Cr (III), Cu (II) and Pb (II) in tea infusions using AgNPs-modified resin combined with laser-induced breakdown spectroscopy.

The detection of heavy metals in tea infusions is important because of the potential health risks associated with their consumption. Existing highly sensitive detection methods pose challenges because they are complicated and time-consuming. In this study, we developed an innovative and simple method using Ag nanoparticles-modified resin (AgNPs-MR) for pre-enrichment prior to laser-induced breakdown spectroscopy for the simultaneous analysis of Cr (III), Cu (II), and Pb (II) in tea infusions. Signal enhancement using AgNPs-MR resulted in amplification with limits of detection of 0.22 µg L-1 for Cr (III), 0.33 µg L-1 for Cu (II), and 1.25 µg L-1 for Pb (II). Quantitative analyses of these ions in infusions of black tea from various brands yielded recoveries ranging from 83.3% to 114.5%. This method is effective as a direct and highly sensitive technique for precisely quantifying trace concentrations of heavy metals in tea infusions.

Rapid Authentication and Detection of Olive Oil Adulteration Using Laser-Induced Breakdown Spectroscopy.

The adulteration of olive oil is a crucial matter for food safety authorities, global organizations, and consumers. To guarantee olive oil authenticity, the European Union (EU) has promoted the labeling of olive oils with the indices of Protected Designation of Origin (PDO) and Protected Geographical Identification (PGI), while food security agencies are also interested in newly emerging technologies capable of operating reliably, fast, and in real-time, either in situ or remotely, for quality control. Among the proposed methods, photonic technologies appear to be suitable and promising for dealing with this issue. In this regard, a laser-based technique, namely, Laser-Induced Breakdown Spectroscopy (LIBS), assisted via machine learning tools, is proposed for the real-time detection of olive oil adulteration with lower-quality oils (i.e., pomace, soybean, sunflower, and corn oils). The results of the present work demonstrate the high efficiency and potential of the LIBS technique for the rapid detection of olive oil adulteration and the detection of adulterants.

Evaluation of medicinal plants using laser-induced breakdown spectroscopy (LIBS) combined with chemometric techniques.

Medicinal plants play a vital role in herbal medical field and allopathic medicine field industry. Chemical and spectroscopic studies of Taraxacum officinale, Hyoscyamus niger, Ajuga bracteosa, Elaeagnus angustifolia, Camellia sinensis, and Berberis lyceum are conducted in this paper by using a 532-nm Nd:YAG laser in an open air environment. These medicinal plant's leaves, roots, seed, and flowers are used to treat a range of diseases by the locals. It is crucial to be able to distinguish between beneficial and detrimental metal elements in these plants. We demonstrated how various elements are categorized and how roots, leaves, seeds and flowers of same plants differ from each other on the basis of elemental analysis. Furthermore, for classification purpose, different classification models, partial least square discriminant analysis (PLS-DA), k-nearest neighbors (kNN), and principal component analysis (PCA) are used. We found silicon (Si), aluminum (Al), iron (Fe), copper (Cu), calcium (Ca), magnesium (Mg), sodium (Na), potassium (K), manganese (Mn), phosphorous (P), and vanadium (V) in all of the medicinal plant samples with a molecular form of carbon and nitrogen band. We detected Ca, Mg, Si, and P as primary components in all of the plant samples, as well as V, Fe, Mn, Al, and Ti as essential medicinal metals, and additional trace elements like Si, Sr, and Al. The result's findings show that the PLS-DA classification model with single normal variate (SNV) preprocessing method is the most effective classification model for different types of plant samples. The average correct classification rate obtained for PLS-DA with SNV is 95%. Moreover, laser-induced breakdown spectroscopy (LIBS) was successfully employed to perform rapid, sensitive, and quantitative trace element analysis on medicinal herbs and plant samples.

Fast Detection of Heavy Metal Content in Fritillaria thunbergii by Laser-Induced Breakdown Spectroscopy with PSO-BP and SSA-BP Analysis.

Fast detection of heavy metals is important to ensure the quality and safety of herbal medicines. In this study, laser-induced breakdown spectroscopy (LIBS) was applied to detect the heavy metal content (Cd, Cu, and Pb) in Fritillaria thunbergii. Quantitative prediction models were established using a back-propagation neural network (BPNN) optimized using the particle swarm optimization (PSO) algorithm and sparrow search algorithm (SSA), called PSO-BP and SSA-BP, respectively. The results revealed that the BPNN models optimized by PSO and SSA had better accuracy than the BPNN model without optimization. The performance evaluation metrics of the PSO-BP and SSA-BP models were similar. However, the SSA-BP model had two advantages: it was faster and had higher prediction accuracy at low concentrations. For the three heavy metals Cd, Cu and Pb, the prediction correlation coefficient (Rp2) values for the SSA-BP model were 0.972, 0.991 and 0.956; the prediction root mean square error (RMSEP) values were 5.553, 7.810 and 12.906 mg/kg; and the prediction relative percent deviation (RPD) values were 6.04, 10.34 and 4.94, respectively. Therefore, LIBS could be considered a constructive tool for the quantification of Cd, Cu and Pb contents in Fritillaria thunbergii.

Specialty and high-quality coffee: discrimination through elemental characterization via ICP-OES, ICP-MS, and ICP-MS/MS of origin, species, and variety.

BACKGROUND: This study aimed to establish the elemental profiling and origin combined with the genetic asset of coffee samples collected from major coffee-producing countries. A total of 76 samples were analysed for 41 elements using inductively coupled plasma-optical emission spectroscopy (ICP-OES), inductively coupled plasma-mass spectrometry (ICP-MS), and inductively coupled plasma-triple quadrupole mass spectrometry (ICP-MS/MS). The mineral composition of the silver skin detachment during the roasting process was also evaluated to verify the loss of minerals during roasting, differences in composition with beans, and between species. RESULTS: Application of linear discriminant analysis provided models with an accuracy of 93.3% for continents, 97.8% for countries of cultivation, and 100% for species. Discrimination between Arabica, Canephora coffee, and Eugenoides, and different varieties of Arabica species were identified in both models with calcium (Ca), barium (Ba), cadmium (Cd), rubidium (Rb), and strontium (Sr) as significant discriminant elements. Rb, Sr, sulphur (S), and thulium (Tm) were significant discriminant elements in both models for geographical distinction at different scales. Most of the elements had significantly higher values in silver skin than those in roasted coffee at different magnitudes, with exceptions of P and Rb. CONCLUSION: In summary, determination of mineral elements, processed by multivariate statistical analysis, was demonstrated to be discriminant for different coffee species. Linear discriminant analysis of the elemental analysis of samples from the seven major producing countries provided a reliable prediction model. Elemental analysis of major and minor elements is relatively easy and can be used together with other traceability systems and sensory evaluations to authenticate the origin of roasted coffee, different species, and varieties. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Advanced techniques in edible oil authentication: A systematic review and critical analysis.

Adulteration of edible substances is a potent contemporary food safety issue. Perhaps the overt concern derives from the fact that adulterants pose serious ill effects on human health. Edible oils are one of the most adulterated food products. Perpetrators are adopting ways and means that effectively masks the presence of the adulterants from human organoleptic limits and traditional oil adulteration detection techniques. This review embodies a detailed account of chemical, biosensors, chromatography, spectroscopy, differential scanning calorimetry, non-thermal plasma, dielectric spectroscopy research carried out in the area of falsification assessment of edible oils for the past three decades and a collection of patented oil adulteration detection techniques. The detection techniques reviewed have some advantages and certain limitations, chemical tests are simple; biosensors and nuclear magnetic resonance are rapid but have a low sensitivity; chromatography and spectroscopy are highly accurate with a deterring price tag; dielectric spectroscopy is rapid can be portable and has on-line compatibility; however, the results are susceptible to variation of electric current frequency and intrinsic factors (moisture, temperature, structural composition). This review paper can be useful for scientists or for knowledge seekers eager to be abreast with edible oil adulteration detection techniques.

Development of microparticles and microparticulated tablets containing piperine

Abstract Piper nigrum (black pepper) is used in Indian traditional medicine and its main alkaloid, Piperine (PIP), presents antioxidant, antitumor and neuroprotective pharmacological properties. This substance is insoluble in aqueous media and can irritate the gastrointestinal tract. Aiming to avoid these inconvenient characteristics and enable PIP oral administration, this study suggested the PIP microencapsulation through the emulsion-solvent evaporation method and the preparation of microparticulated tablets by direct compression. An UV-spectroscopy method was validated to quantify PIP. Microparticles and microparticulated tablets were successfully obtained and the microparticles exhibited excellent flow. The scanning electron microscopy images showed that PIP microparticles were intact after compression. The in vitro release showed a controlled release of PIP from microparticles and PIP microparticles from tablets in comparison to PIP and PIP tablets. The release profiles of PIP microparticles and the microparticulated tablets were similar. Therefore, tablets containing PIP microparticles are promising multiparticulated dosage forms because a tablet allows microparticles administration and the intact ones promote a controlled release, decreasing its irritating potential on the mucosa.

Tutorial on the instrumentation of sum frequency generation vibrational spectroscopy: Using a Ti:sapphire based system as an example.

Sum frequency generation vibrational spectroscopy (SFG-VS) is an intrinsically surface-selective vibrational spectroscopic technique based on the second-order nonlinear optical process. Since its birth in the 1980s, SFG-VS has been used to solve interfacial structure and dynamics in a variety of research fields including chemistry, physics, materials sciences, biological sciences, environmental sciences, etc. Better understanding of SFG-VS instrumentation is no doubt an essential step to master this sophisticated technique. To address this need, here we will present a Tutorial with respect to the classification, setup layout, construction, operation, and data processing about SFG-VS. We will focus on the steady state Ti:sapphire based broad bandwidth SFG-VS system and use it as an example. We hope this Tutorial is beneficial for newcomers to the SFG-VS field and for people who are interested in using SFG-VS technique in their research.

Effect of deuteration on a phosphatidylcholine lipid monolayer structure: New insights from vibrational sum-frequency generation spectroscopy.

We used vibrational sum-frequency generation (VSFG) spectroscopy to elucidate the possible effect of various levels of isotopic substitution (H/D) on the properties of the DPPC monolayer by probing DPPC/D2O interface. We found that deuteration of the choline group has a great impact on monolayer properties, while monolayers with deuterated alkyl chains do not exhibit any differences under our experimental conditions. In addition, deuteration of the choline group strongly affected the hydration of the phosphate group. We showed by probing symmetric stretching vibration of phosphate group that denser packing only slightly reduced the hydration of DPPC-d13 and DPPC-d75 monolayers. Moreover, addition of calcium ions, which generally cause a marked dehydration of the lipid monolayer, had no effect on lipid monolayers with deuterated choline group. We proposed that one way to explain this experimental finding could be deuteration induced changes in the structure of lipid's choline group, resulting in a well-hydrated but Ca2+ ion blocking structure. These results have important implications for various spectroscopic techniques, which commonly use deuteration of phospholipids to circumvent overlapping between vibrational bands.

Estimation of porcine pancreas optical properties in the 600-1100 nm wavelength range for light-based therapies.

This work reports the optical properties of porcine pancreatic tissue in the broad wavelength range of 600-1100 nm. Absorption and reduced scattering coefficients (µa and µs') of the ex vivo pancreas were obtained by means of Time-domain Diffuse Optical Spectroscopy. We have investigated different experimental conditions-including compression, repositioning, spatial sampling, temporal stability-the effect of the freezing procedure (fresh vs frozen-thawed pancreas), and finally inter-sample variability. Good repeatability under different experimental conditions was obtained (median coefficient of variation less than 8% and ~ 16% for µa and µs', respectively). Freezing-thawing the samples caused an irreversible threefold reduction of µs' and no effect on µa. The absorption and reduced scattering spectra averaged over different samples were in the range of 0.12-0.74 cm-1 and 12-21 cm-1 with an inter-sample variation of ~ 10% and ~ 40% for µa and µs', respectively. The calculated effective transport coefficient (µeff) for fresh pancreatic tissue shows that regions between 800-900 nm and 1050-1100 nm are similar and offer the lowest tissue attenuation in the considered range (i.e., µeff ranging from 2.4 to 2.7 cm-1). These data, describing specific light-pancreas interactions in the therapeutic optical window for the first time, provide pivotal information for planning of light-based thermotherapies (e.g., laser ablation) and instruction of light transport models for biophotonic applications involving this organ.

Response surface methodology assisted development of a simplified sample preparation procedure for the multielement (Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn) analysis of different coffee brews by means of inductively coupled plasma optical emission spectrometry.

The Box-Behnken response surface design together with the individual desirability functions were used to develop the new and greenish sample preparation procedure of coffee brews prior to their multielement (Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn) analysis by inductively coupled plasma optical emission spectrometry (ICP OES). The developed procedure required only 2-fold dilution of the samples with a 1.8 mol L-1 HNO3 solution and then, the sonication of the resulting samples solutions for 8 min at room temperature. The proposed method was precise (0.6-7.5% as RSD), true (relative errors changing from -5.2% to +4.6%) and guaranteed the limits of detection (LODs) of the studied elements between 0.1 and 5 ng g-1. Finally, this simplified ICP OES based method was applied for the multielement analysis of brews of different Arabica coffees as well as those prepared with seldomly reported devices, i.e., dripper, slow dripper, French press, aeropress and syphon.

Systematic assessment of process analytical technologies for biologics.

The application of process analytical technology (PAT) for biotherapeutic development and manufacturing has been employed owing to technological, economic, and regulatory advantages across the industry. Typically, chromatographic, spectroscopic, and/or mass spectrometric sensors are integrated into upstream and downstream unit operations in in-line, on-line, or at-line fashion to enable real-time monitoring and control of the process. Despite the widespread utility of PAT technologies at various unit operations of the bioprocess, a holistic business value assessment of PAT has not been well addressed in biologics. Thus, in this study, we evaluated PAT technologies based on predefined criteria for their technological attributes such as enablement of better process understanding, control, and high-throughput capabilities; as well as for business attributes such as simplicity of implementation, lead time, and cost reduction. The study involved an industry-wide survey, where input from subject matter industry experts on various PAT tools were collected, assessed, and ranked. The survey results demonstrated on-line liquid Chromatography (LC), in-line Raman, and gas analysis techniques are of high business value especially at the production bioreactor unit operation of upstream processing. In-line variable path-length UV/VIS measurements (VPE), on-line LC, multiangle light scattering (MALS), and automated sampling are of high business value in Protein A purification and polishing steps of the downstream process. We also provide insights, based on our experience in clinical and commercial manufacturing of biologics, into the development and implementation of some of the PAT tools. The results presented in this study are intended to be helpful for the current practitioners of PAT as well as those new to the field to gauge, prioritize and steer their projects for success.

Phytochemical Investigation of the Roots of Ipomoea asarifolia and Antiproliferative Activity of the Isolated Compounds against Multiple Myeloma Cells.

Ipomoea asarifolia is a herbaceous plant belonging to the family Convolvulaceae and is native to tropical regions of Africa, America, and Asia. A dichloromethane root extract showed antiproliferative activity against multiple myeloma cells (RPMI 8226). The phytochemical investigation led to the isolation of 15 compounds. Compounds 1-4, named (4S,8S)-1-(furan-3-yl)-9-hydroxy-4,8-dimethylnonane-1,6-dione, isoferulic acid hexadecyl ester, caffeic acid hexadecyl ester, and asarifolin I, respectively, are described for the first time. The structures of these molecules were established from their NMR, UV, IR spectroscopic, and MS data. 4-Hydroxycinnamic acid hexadecyl ester (5), 4-hydroxycinnamic acid octadecyl ester (6), 4-hydroxycinnamic acid eicosyl ester (7), caffeic acid octadecyl ester (8), pescapreins III, IV, XXI, XXIII, XXV, and XXVI (9-14), and stoloniferin III (15) were also isolated. All compounds were tested against a multiple myeloma cell line (RPMI 8226). When their IC50 value was lower than 10 µM, the compounds were also tested against two other multiple myeloma cell lines, MM.1S and MM.1R. Compound 3 was the most potent, with an IC50 value of 3.0 µM against RPMI 8226 cells.

Investigation on the Q-markers of Bushen Huoxue Prescriptions for DR treatment based on chemometric methods and spectrum-effect relationship.

ETHNOPHARMACOLOGICAL RELEVANCE: Diabetic retinopathy (DR) is a kind of complex complication of late diabetes mellitus with high incidence and risk of blindness. Bushen Huoxue Prescription (BHP), which consists of Rehmanniae radix (RR), Salviae miltiorrhizae radix et rhizoma (SMRR), Ginseng radix et rhizome (GRR) and Puerariae lobatae radix (PLR), has an active effect on the treatment of DR. However, the quality markers (Q-markers) of BHP are not entirely clear. PURPOSE: This study aimed to screen the Q-markers of BHP for DR treatment based on the establishment of spectrum-effect relationship and verified experiment. MATERIALS AND METHODS: In this study, 12 BHP samples (S1-S12) for fingerprint analysis and pharmacological evaluation were prepared according to a four-factor and twelve-level uniform design. High performance liquid chromatography-ultraviolet detector-evaporative light scattering detector (HPLC-UV-ELSD) was employed to analyze the fingerprint on the basis of the characteristics of BHP components. The evaluation of sample similarity was carried out by similarity analysis (SA) and hierarchical cluster analysis (HCA). The pharmacological indicators, including expression of vascular endothelial growth factor (VEGF) and hypoxia-inducible factor-1α (HIF-1α) in the retina of Sprague Dawley (SD) rats induced by streptozotocin (STZ), were detected by enzyme-linked immunosorbent assay (ELISA). Besides, the spectrum-effect relationship between common peaks of fingerprints and the pharmacological results was investigated by partial least squares regression (PLSR) and canonical correlation analysis (CCA). The results of spectrum-effect relationship were verified by the expression of VEGF and HIF-1α on primary culture retinal Müller cells induced by hyperglycemia and hypoxia. RESULTS: In the HPLC-UV-ELSD fingerprint, 23 common peaks in UV and 14 common peaks in ELSD were identified. The pharmacological results indicated that the expression of VEGF and HIF-1α in the retina of SD rats was inhibited by 12 BHP samples to varying degrees compared with the model group. Based on SA and heatmap of HCA, S4 and S8 were clearly distinguished from other samples. The results of PLSR and CCA revealed that the contents of puerarin, daidzin, salvianolic acid B and ginsenoside Rb1 were inversely correlated with the expression of VEGF and HIF-1α. Hence, the four compounds may be the main active components to prevent and treat DR. The results of intervention on primary culture retinal Müller cells showed that puerarin, daidzin, salvianolic acid B, and ginsenoside Rb1 can significantly inhibit the expression of VEGF and HIF-1α. CONCLUSIONS: The spectrum-effect relationship of BHP was successfully established, and the Q-markers of BHP for the prevention and treatment of DR were preliminarily confirmed. It provides a feasible method for the research of quality control.

Inhibition of BACE1 and amyloid ß aggregation by polyketide from Streptomyces sp.

Alzheimer's disease (AD) causes cognitive impairment in the elderly and is a severe problem worldwide. One of the major reasons for the pathogenesis of AD is thought to be due to the accumulation of amyloid beta (Aß) peptides that result in neuronal cell death in the brain. In this study, bioassay-guided fractionation was performed to develop seed compounds for anti-AD drugs that can act as dual inhibitors of BACE1 and Aß aggregation from secondary metabolites produced by Streptomyces sp. To improve the solubility, the crude extracts were methylated with trimethylsilyl (TMS) diazomethane and then purified to yield polyketides 1-5, including the new compound 1. We synthesized the compounds 6 and 7 (original compounds 2 and 3, respectively), and their activities were evaluated. KS-619-1, the demethylated form of 4 and 5, was isolated and evaluated for its inhibitory activity. The IC50 values for BACE1 and Aß aggregation were found to be 0.48 and 1.1 µM, respectively, indicating that KS-619-1 could be a lead compound for the development of therapeutic agents for AD.

Multifaceted phytogenic silver nanoparticles by an insectivorous plant Drosera spatulata Labill var. bakoensis and its potential therapeutic applications.

The current investigation highlights the green synthesis of silver nanoparticles (AgNPs) by the insectivorous plant Drosera spatulata Labill var. bakoensis, which is the first of its kind. The biosynthesized nanoparticles revealed a UV visible surface plasmon resonance (SPR) band at 427 nm. The natural phytoconstituents which reduce the monovalent silver were identified by FTIR. The particle size of the Ds-AgNPs was detected by the Nanoparticle size analyzer confirms that the average size of nanoparticles was around 23 ± 2 nm. Ds-AgNPs exhibit high stability because of its high negative zeta potential (- 34.1 mV). AFM studies also revealed that the Ds-AgNPs were spherical in shape and average size ranges from 10 to 20 ± 5 nm. TEM analysis also revealed that the average size of Ds-AgNPs was also around 21 ± 4 nm and the shape is roughly spherical and well dispersed. The crystal nature of Ds-AgNPs was detected as a face-centered cube by the XRD analysis. Furthermore, studies on antibacterial and antifungal activities manifested outstanding antimicrobial activities of Ds-AgNPs compared with standard antibiotic Amoxyclav. In addition, demonstration of superior free radical scavenging efficacy coupled with potential in vitro cytotoxic significance on Human colon cancer cell lines (HT-29) suggests that the Ds-AgNPs attain excellent multifunctional therapeutic applications.

Quantification of Corn Adulteration in Wet and Dry-Processed Peaberry Ground Roasted Coffees by UV-Vis Spectroscopy and Chemometrics.

In this present research, a spectroscopic method based on UV-Vis spectroscopy is utilized to quantify the level of corn adulteration in peaberry ground roasted coffee by chemometrics. Peaberry coffee with two types of bean processing of wet and dry-processed methods was used and intentionally adulterated by corn with a 10-50% level of adulteration. UV-Vis spectral data are obtained for aqueous samples in the range between 250 and 400 nm with a 1 nm interval. Three multivariate regression methods, including partial least squares regression (PLSR), multiple linear regression (MLR), and principal component regression (PCR), are used to predict the level of corn adulteration. The result shows that all individual regression models using individual wet and dry samples are better than that of global regression models using combined wet and dry samples. The best calibration model for individual wet and dry and combined samples is obtained for the PLSR model with a coefficient of determination in the range of 0.83-0.93 and RMSE below 6% (w/w) for calibration and validation. However, the error prediction in terms of RMSEP and bias were highly increased when the individual regression model was used to predict the level of corn adulteration with differences in the bean processing method. The obtained results demonstrate that the use of the global PLSR model is better in predicting the level of corn adulteration. The error prediction for this global model is acceptable with low RMSEP and bias for both individual and combined prediction samples. The obtained RPDp and RERp in prediction for the global PLSR model are more than two and five for individual and combined samples, respectively. The proposed method using UV-Vis spectroscopy with a global PLSR model can be applied to quantify the level of corn adulteration in peaberry ground roasted coffee with different bean processing methods.

Chemometric approach to find relationships between physiological elements and elements causing toxic effects in herb roots by ICP-MS.

In this paper 13 elements, both physiological and causing toxic effects, were determined by inductively coupled plasma mass spectrometry in roots of 26 species of herbs used in Traditional Chinese Medicine. The herbs were purchased from online shop in two batches 1 year apart to verify the variability of elemental content in time. The multivariate statistical methods-multiple regression, canonical variates and interaction effect analysis-were applied to interpret the data and to show the relationships between elements and two batches of herb roots. The maximum permissible concentration of Cd (0.3 mg kg-1) was exceeded in 7 herb roots which makes 13% of all specimens. The multiple regression analysis revealed the significant relationships between elements: Mg with Sr; V with Pb, As and Ba; Mn with Pb; Fe with As and Ba; Co with Ni and Sr, Cu with Pb, Cd and As; Zn with Pb, Cd, As and Ba. The canonical variates analysis showed that the statistical inference should not be based solely on the type of herb or number of batch because of the underlying interaction effects between those two variables that may be a source of variability of the content of determined elements.

Magnetic solid-phase extraction of high molecular weight peptides using stearic acid-functionalized magnetic hydroxyapatite nanocomposite: determination of some hypothalamic agents in biological samples.

Therapeutic peptides have an important effect on physiological function and human health, so it is momentous to quantify and detect low levels of these biomolecules in biological samples for treatment and diagnostic purposes. In the present study, an efficient magnetic solid-phase extraction (MSPE) method was developed based on stearic acid-functionalized magnetic hydroxyapatite nanocomposite (MHAP/SA) as a novel and cost-effective adsorbent for extraction of five hypothalamic-related peptides (goserelin, octreotide, triptorelin, somatostatin, and cetrorelix) from biological samples. To characterize the morphology and physicochemical properties of MHAP/SA, Fourier transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDS), field emission scanning microscopy (FE-SEM), CHNS elemental analysis, Brunauer-Emmett-Teller (BET), and vibrating sample magnetometry (VSM) were applied. Under optimum conditions, the proposed method (MSPE-HPLC-UV) represented favorable linearity with R2 ≥ 0.9987, suitable intra- and inter-day precisions (RSD ≤ 6.9% and RSD ≤ 8.1%, respectively, n = 3), and limits of detection and quantification in the range of 0.75-1.12 ng mL-1 and 2.50-3.75 ng mL-1, respectively. Eventually, the proposed method was used for the extraction and quantification of target therapeutic peptides in plasma and urine samples, and satisfactory relative recoveries were achieved in the range of 90.6-110.3%.

In-line monitoring and endpoint determination of percolation process of herbal medicine using ultraviolet spectroscopy combined with convolutional neural network.

OBJECTIVES: As a common step in the herbal medicine production process, percolation usually lacks effective process monitoring methods and is often conducted with fixed process parameters. In this study, an in-line ultraviolet (UV) spectroscopy was used for monitoring the Caulis Sinomenii percolation process. METHODS: The spectra and concentration data of 156 percolation samples from five batches were collected. Convolutional neural networks (CNNs) were used to develop quantitative calibration models. The mean squared error (MSE), mean absolute percentage error (MAPE) and mean absolute error (MAE) were compared to select the proper loss function for developing the CNN models. Meanwhile, partial least square regression (PLSR) was also used to develop calibration models for performance comparison. KEY FINDINGS: The CNN models with MAPE or MAE as the loss function could provide accurate predictions for all samples. However, CNN models adopting MSE as the loss function tended not to predict low-concentration samples accurately. The CNN models mostly achieved satisfactory results without any preprocessing techniques and surpassed PLSR models in all the performance metrics. CONCLUSIONS: An in-line UV spectroscopy system combining the CNN algorithm was implemented to monitor the percolation process of Caulis Sinomenii. The system can accurately determine the endpoint of the percolation process.