Analysis Method Research Articles

A fully validated LC‑MS/MS method for quantifyingbevacizumab in plasma samples from patients with NSCLC and its implications in therapeutic drug monitoring.

Given the increasing use of bevacizumab in combinatorial drug therapy for a multitude of different cancer types, there is a need for therapeutic drug monitoring to analyze the possible correlation between drug trough concentration, and therapeutic effect and adverse reactions. An ultra-performance liquid chromatography tandem-mass spectrometry method was then developed and validated to determine bevacizumab levels in human plasma samples. Chromatographic separation was achieved on a Shimadzu InertSustainBio C18 HP column, whereas subsequent mass spectrometric analysis was performed using a Shimadzu 8050CL triple quadrupole mass spectrometer equipped with an electro-spray ionization source in the positive ion mode. In total, three multiple reaction monitoring transitions of each of the surrogate peptides were chosen with 'FTFSLDTSK' applied as the quantification peptide whereas 'VLIYFTSSLHSGVPSR' and 'STAYLQMNSLR' were designated as the verification peptides using the Skyline software. This analytical method was then fully validated, with specificity, linearity, lower limit of quantitation, accuracy, precision, stability, matrix effect and recovery calculated. The linearity of this method was developed to be within the concentration range 5-400 µg/ml for bevacizumab in human plasma. Subsequently, eight patients with non-small cell lung cancer (NSCLC) were recruited and injected with bevacizumab over three periods of treatment to analyze their steady-state trough concentration and differences. To conclude, the results of the present study suggest that bevacizumab can be monitored in a therapeutic setting in patients with NSCLC.

Determination of polycyclic aromatic hydrocarbons, phthalate esters, alkylphenols and alkyphenol ethoxylates in sediment using simultaneous focused ultrasound solid–liquid extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography

The study presents a simple and non-laborious method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs), 2 phthalate esters (PEs), 2 alkylphenols (APs) and 4 alkylphenol ethoxylates (APEOs) in sediment. The method employs sample preparation combining focused ultrasound solid–liquid extraction (FUSLE) and in situ clean-up followed by liquid chromatography with fluorescence and ultraviolet detection. Extraction of 0.5 g sediment samples with 7 mL acetone in the presence of activated silica (0.5 g) and powdered copper (0.2 g) using an ultrasonic probe for 1 min resulted in recoveries of target analytes ≥ 78 %. The analytical method was classified as “acceptable green analysis” by the analytical Eco-Scale assessment (AESA) and scored 0.54 in the AGREEprep greenness assessment for sample preparation. Matrix-matched calibration was used to quantify analytes with a linear range for PAHs 2–1000 ng g–1, for PEs 100–5000 ng g–1 and for APs and APEOs 40–2000 ng g–1 dry weight. The reached limits of quantification (LOQ) for PAHs ranged from 1.1 to 3.1 ng g−1, for PEs from 122 to 124 ng g−1, for APs from 40 to 51 ng g−1 and for APEOs from 36 to 53 ng g−1. The applicability of the method was demonstrated by the analysis of real sediment samples and natural matrix certified reference material.

QbD Assisted Development and Validation of UV Spectroscopic Method in Estimation of Silymarin

Background: Silymarin is a flavonoid utilised in liver dysfunction for years; new studies have emphasised its potential utility as a therapy for nanoparticulate targeting in many other disorders. In order to establish the product quality of such compounds, researchers have been trying to develop a robust method of analysis, but the methods developed till now are too expensive and time-consuming. Here we proposed quality by design-assisted development and validation of the UV spectroscopic method using Design-Expert® software in the estimation of Silymarin for fabrication of nanoparticulate formulations, which is simple, accurate, cost-effective and non-tedious. Aim: The proposed method is a simple, new, robust, accurate, and precise UV visible spectroscopic technique for estimating silymarin produced in nano-formulations utilising an analytical quality by design (AQbD) approach. Methods: A UV spectrophotometric technique was established, as maximum absorption (287.7) was measured using a Shimadzu UV-1800 double-beam UV visible spectrophotometer. The characterization of silymarin was done by melting point, DSC and FTIR techniques. The two critical method variables chosen were scanning speed and sample interval to be analysed by the design of experiment methodology utilizing the central composite design principle, which shows robustness and optimized technique involved in this work. Results: The spectroscopy technique was developed and validated as per International Conference of Harmonization recommendations. The Beer's-Lambert rule was followed in a series of 2-12 μg/ml dilution increments, with a correlation value of R2 = 0.999. The method's linearity was shown to be excellent across the concentration range. The percent recovery of the current method approach was determined to be within the confidential limitations, i.e., less than 2% expressed as % RSD, and the methodology was proved to be precise at inter and intraday variations (% RSD). The LOD and LOQ were found to be 0.264 μg/ml and 0.801 μg/ml which were also determined correctly. During specificity testing, no interfering peaks were found. Conclusion: This UV approach has been used successfully to determine the quantity of silymarin present in the nanoparticulate formulation, which can be used for testing its other pharmaceutical dosage forms.

Extraction Optimization, Structure Analysis and Antioxidant Activity of Polysaccharide from Sanghuangporus baumii

Introduction: In this study, we optimized the extraction process, analyzed the structure and assessed the antioxidant activity of Sanghuangporus baumii polysaccharide (SBP). The present results provide important information for the Sanghuangporus baumii polysaccharides in potential natural antioxidant effects. Background: The extraction and structural analysis of polysaccharides from Sanghuangporus has gained significant attention in the fields of chemistry, medicine, and life sciences. There is great significance in maximizing the extraction of polysaccharides from Sanghuangporus and developing their potential products in a scientific and rational manner. Objective: The study was designed to establish an efficient and practical extraction process for SBP, and then investigated the structure and the antioxidant activity. Methods: The Response Surface Methodology (RSM) based on Box-Behnken design was used to explore the ultrasound-assisted extraction of SBP, and the structure of SBP was studied by ultraviolet spectroscopy, infrared spectroscopy and other instrumental analysis methods. The total antioxidant capacity of SBP was studied by the Ferric Reducing Ability of Plasma (FRAP) method, and the scavenging capacity of ABTS+·, DPPH· and OH· was carried out as the index to investigate its antioxidant activity in vitro. Results: The statistical analysis results showed that the optimal conditions for extracting SBP were an ultrasound time of 20.74 min, ultrasound power of 268.40 W and material-liquid ratio of 1:25.71. Under optimal conditions, the experimental yield of SBP was 3.36 ± 0.01%. The RSM optimization process was applied to the experiment of complex enzyme extraction of SBP, and the yield increased to 4.72 ± 0.03%. Structural analysis showed that SBP mainly consisted of glucose, a small amount of mannose and galactose, and the molecular weight distribution was uneven, mainly concentrating in the three parts of 24.5,6.4,2.5 kDa. Moreover, SBP exhibited dose-dependent and strong reducing power and radical scavenging activity. For DPPH·, ABTS+· and OH· radical scavenging assays, IC50 values were 1.505 ± 0.050 mg/ml, 0.065 ± 0.036 mg/ml and 0.442 ± 0.007 mg/ml, respectively. Conclusion: In the present study, a β-linked heteroglucan (SBP) was extracted using the optimized process combining enzymes from the fruiting bodies of Sanghuangporus baumii. SBP exhibited effective and dose-dependent antioxidant activities. Our findings were of great value in terms of developing polysaccharides with potential natural antioxidants.

Verification of analytical performance of Unsaturated iron binding capacity (UIBC) assay on the Abbott Alinity ci®: Experience of the central laboratory of Mohammed VI University Hospital of Oujda

The verification of analytical methods is a requirement outlined by the International Organization for Standardization (ISO). This process involves evaluating the performance of an analytical method according to a well-defined protocol and subsequently comparing it with pre-established analytical objectives. In our study, we conducted an evaluation of the analytical performance of the unsaturated iron binding capacity assay using the Abbott kit on the Alinity CI analyzer in the biochemistry laboratory of Mohammed VI University Hospital in Oujda. The methodology employed adheres to the recommendations of the French accreditation committee (COFRAC) accreditation technical guide SH GTA 04, focusing on the assessment of reproducibility and repeatability. Overall, the results obtained from the study are considered satisfactory and align with the acceptability criteria recommended by the supplier. It's important to note that the accuracy and reliability of examination results are influenced not only by laboratory personnel, equipment, and environmental conditions, but also by the methods utilized and their eventual validation or verification.

Robust high-performance thin-layer chromatography (HPTLC) method for stability assessment and simultaneous quantification of epigallocatechin-3-gallate and rosmarinic acid in lipid-based nanoparticles and biological matrices.

Skin cancer poses a significant health risk globally, necessitating effective and safe therapeutic interventions. Epigallocatechin-3-gallate (EGCG) from green tea and rosmarinic acid (RA) from herbs like rosemary offer promising anticancer properties. Combining these compounds may enhance their effectiveness, prompting the need for a reliable analytical method to quantify them. Herein, we present the development and validation of a high-performance thin-layer chromatography (HPTLC) method for concurrent quantification of EGCG and RA in lipid-based nanoparticles and biological samples. The method underwent optimisation through design of experiments (DoE), resulting in the establishment of robust chromatographic conditions. The separation process utilised aluminium HPTLC plates coated with silica gel 60 F254 as the stationary phase, with the mobile phase comprising ethyl acetate, toluene, formic acid, and methanol in a ratio of 4:4:1:1 v/v. The retention factor (Rf) values obtained were 0.38 for EGCG and 0.61 for RA. The method demonstrated linearity over a range of 100-500 ng/band for both compounds with excellent correlation coefficients. Limits of detection and quantification were determined, indicating high sensitivity. Precision evaluations revealed relative standard deviation below 2%, ensuring method reproducibility. Recovery assays in lipid-based nanoparticles, plasma, and urine samples demonstrated excellent recoveries (96.2%-102.1%). Forced degradation studies revealed minimal degradation under various stress conditions, with photolytic degradation showing the least impact. The developed HPTLC method offers a rapid, sensitive, and reliable approach for quantifying EGCG and RA, laying the groundwork for their further investigation as anticancer agents alone and in combination therapies.

Enhanced Detection of Estrogen-like Compounds by Genetically Engineered Yeast Sensor Strains

The release of endocrine-disrupting compounds (EDCs) to the environment poses a health hazard to both humans and wildlife. EDCs can activate or inhibit endogenous endocrine functions by binding hormone receptors, leading to potentially adverse effects. Conventional analytical methods can detect EDCs at a high sensitivity and precision, but are blind to the biological activity of the detected compounds. To overcome this limitation, yeast-based bioassays have previously been developed as a pre-screening method, providing an effect-based overview of hormonal-disruptive activity within the sample prior to the application of analytical methods. These yeast biosensors express human endocrine-specific receptors, co-transfected with the relevant response element fused to the specific fluorescent protein reporter gene. We describe several molecular manipulations of the sensor/reporter circuit in a Saccharomyces cerevisiae bioreporter strain that have yielded an enhanced detection of estrogenic-like compounds. Improved responses were displayed both in liquid culture (96-well plate format) as well as in conjunction with sample separation using high-performance thin-layer chromatography (HPTLC). The latter approach allows for an assessment of the biological effect of individual sample components without the need for their chemical identification at the screening stage.

How Do Operating Room Nurse Students Experience the Learning Environment in the Operating Room?

Please note this article was first published in Norwegian. You can read the Norwegian article here. Background: There is little research-based knowledge about how operating room nursing students experience the learning environment in an operating room. Results from international studies indicate that structural challenges such as time pressure, high demands for efficiency, and a minimum of time delegated to guidance are all characteristic of the learning environment. More insight into how operating room nursing students experience an operating room is an important element for improving the quality of practice studies in a high-tech and time-efficient environment. Aim: The purpose of the study is to describe operating room nursing students’ experiences of their learning environment in operating rooms. Method: The study has a qualitative and descriptive research design, utilizing systematic text condensation as an analytical method. Data was gathered through conducting focus-group interviews with operating room nursing students in their final semester of the nursing education study program. Results: Three main categories were brought up repeatedly by these students: 1) The significance of having supervisors, 2) The unclear responsibility with respect to formal and informal guidance in a multidisciplinary learning environment, and 3) The situation of learning in a complex and unpredictable learning environment. Conclusion: The results provide further insight into operating room nursing students’ experiences of their learning environment in authentic practice studies. The results can be utilized in further improving the learning environment for operating room nursing students.

The Effect of Tax Avoidance on Cost of Debt with Institutional Ownership as a Moderating Variable (Empirical Study of Energy Sector Companies Listed on The IDX 2020-2022)

This research aims to test the effect of tax avoidance on the cost of debt with institutional ownership as a moderating variable. In this research, tax avoidance is measured by the effective tax rate. The population in this research is energy sector companies listed on the Indonesia Stock Exchange for the 2020-2022 period. This type of research is quantitative research. The sample in this research was obtained using purposive sampling, namely selecting samples using predetermined criteria. Based on the purposive sampling method, 57 samples were obtained from 82 energy sector companies listed on the Indonesia Stock Exchange for the 2020-2022 period. The analytical methods used are simple linear regression analysis, Moderated Regression Analysis, partial test (t), and coefficient of determination test (R2) using the SPSS version 16 program. The results of this research show that tax avoidance has a significant negative influence on cost of debt. Institutional ownership can strengthen the tax avoidance and cost of debt variables.

Analytical Solution for the Deformation of Pipe Galleries Adjacent to Deep Excavation

Deep excavations clearly impact adjacent existing properties and threaten their operational safety. Predicting the deformation of existing infrastructure induced by nearby underground construction is the main concern of urban underground development. This paper presents an analytical calculation method for predicting underground pipe gallery deformations induced by adjacent deep excavations. First, the authors assume the existing pipe gallery to be nonexistent in the soil and propose a solution to calculate the excavation-induced vertical movements of the soil at the position of the existing pipe gallery. Thereafter, the authors simplify the existing pipe gallery as an elastic beam on a Winkler foundation to calculate its deformation. Finally, the method is verified by the good agreement found between the calculated result and the field measurement of the construction of the Shanghai Hongqiao CBD project. The proposed analytical method of this work can provide accurate evaluation results for similar engineering projects.

“El embarazo está en la cabeza, no en el útero”: el oráculo del <i>diloggún</i> y el despertar de la fertilidad en la regla de ocha cubana

Religions are often acknowledged for their ability to provoke social, psychological, and physiological transformation, prompting recurrent studies in social and human sciences. Within this analytical domain, understanding ailments and methods of healing through various practices —rituals, cosmologies, and divinations— has been extensively explored. However, research on female reproductive ailments and corresponding intervention methods remains nascent in certain religious denominations, such as African-derived religions like the Regla de Ocha (Santería) in Cuba. The purpose of this article is to shed light on the healing of female reproductive ailments through the diloggún oracle utilized in the Regla de Ocha. Conducted between December 2022 and January 2023 in Santa Marta, Cárdenas, Cuba, our research adopts an ethnographic and narrative approach, placing reflexivity on our experiences at the forefront of our discussions. The research, from which our arguments derive, was conducted between December 2022 and January 2023 in Santa Marta, Cárdenas, Cuba. Methodologically, it adopts an ethnographic and narrative approach, placing reflexivity on our experiences at the forefront of our discussions. Consequently, it not only delineates the processes inherent in the practice of this oracle and its socio-spiritual impacts concerning potential realms of well-being but also advocates for conceptual and theoretical-methodological enhancements regarding healing. The article contributes to the evolving the incipient understanding of the connections between female fertility and healing within the Regla de Ocha and the intricate relationships among well-being, discomfort, and spirituality intrinsic to this religious system.

Investigating the level of vitamin D receptor gene expression in two tumoral and healthy breast tissues in breast cancer patients and its association with prognostic factors.

Breast cancer is one of the most common cancers known among women. This study aimed to investigate the level of vitamin D receptor gene expression in two tumoral and healthy breast tissues in breast cancer patients and its association with prognostic factors. This descriptive cross-sectional study was conducted in 2022 on 50 patients with high suspicion of breast cancer who were candidates for mastectomy and lumpectomy in a learning hospital. From the patients, two tissue samples were prepared, and there was a total of 100 samples. The samples were subjected to H/E staining and evaluated by a pathologist. The presence or absence of malignancy in each sample was confirmed by two pathologists, and HER2/ER/PR indices were determined. Descriptive and analytical statistical methods and SPSS version 22 software were used. The average age of the patients was 51.60 ± 11.22 years old, and the average tumor size was 3.17 ± 1.28. Most tumors were grade 2 (48%). The expression of HER2, ER, and PR was positive in 24, 64, and 54%, respectively. The largest number of cases were in stage 2A. The expression level of vitamin D receptor (VDR) gene in healthy tissue (2.08 ± 1.01) was higher than tumoral tissue (0.25 ± 1.38) (P = 0.001). In tumoral and healthy tissue, VDR expression was not significant according to tumor grade, HER2, ER, PR, LVI, LN, disease stage, age, and tumor size. The expression level of VDR in healthy tissue was significantly higher than tumoral tissue. However, there was no significant relationship between VDR and tumor grade, HER2, ER, PR, LVI, LN, disease stage, age, and tumor size.

HPLC-MS/MS method development and validation for the determination of tetradecapeptide in human plasma

Introduction. The number of peptide drugs being developed and registered has increased in recent years. Therefore, modern analytical approaches and methods are required to determine these substances in biological matrices during pharmacokinetic studies. Peptides are structurally intermediate between small molecules and biopolymers, making it difficult to develop methods for determining them using High Performance Liquid Chromatography with Tandem Mass Spectrometry (HPLC-MS/MS). Peptide derivatization can help achieve optimal chromatographic separation and increase method sensitivity.Aim. To develop and validate a method for the determination of the tetradecapeptide (TDP) threonyl-glutamyl-lysyl-lysyl-arginyl-arginyl-glutamayl-threonyl-valyl-glutamyl-arginyl-glutamyl-lysyl-glutamate in human plasma by HPLC-MS/MS.Materials and methods. The determination of TDP in human plasma was performed by HPLC-MS/MS. Sample preparation included a combination of blood plasma protein precipitation with propionic acid solution in methanol, liquid-liquid extraction with chloroform, and peptide derivatization with propionic anhydride. Internal standard (IS) was threonyl-glutamyl-lysyl-lysyl-arginyl-arginyl-glutamayl-threonyl-leucyl-glutamyl-arginyl-glutamyl-lysyl-glutamate. Chromatographic separation was performed in gradient mode, eluent A was 0.1 % formic acid solution in water, eluent B was 0.1 % formic acid in acetonitrile. Column: Waters XBridge C18, 4.6 × 50 mm, 5 µm. Ionization source was electrospray in positive mode. Multiple reaction monitoring (MRM) transitions for 4-substituted TDP propionate were: 681.30 → 73.95 m/z, 681.30 → 84.00 m/z, 681.30 → 101.90 m/z, 681.30 → 140.10 m/z, and for 4-substituted IS propionate: 686.00 → 74.10 m/z, 686.00 → 84.05 m/z, 686.00 → 102.00 m/z, 686.00 → 140.00 m/z.Results and discussion. Validation of the developed method was carried out in accordance with the requirements of Eurasian Economic Union and the following parameters were determined: selectivity, matrix effect, calibration curve, accuracy and precision, recovery, lower limit of quantification, sample carryover, stability.Conclusion. The method for the determination of TDP in human blood plasma by HPLC-MS/MS was developed and validated. The analytical range was 5.00–1000.00 ng/mL, allowing the method to be used to study TDP pharmacokinetics.

Numbers of prenatal cell-free DNA screens performed: Results of a 2022 CAP exercise.

Determine current analytical methods and number of cell-free (cf) DNA prenatal screening tests performed for common trisomies. The College of American Pathologists 2022-B Noninvasive Prenatal Testing exercise was distributed in December 2022 to 93 participants in 22 countries. Supplemental questions included the number of tests performed in a recent month and the proportion of samples originating outside the United States (US). Eighty-three participants from three continents returned results; 74 (89%) were suitable for the analyses. Nine manufacturer/platform combinations were identified, most commonly Illumina/Nextseq (55%). The most common methodology was whole genome sequencing (76%). Annualized cfDNA tests were 2.80 million, with Asian, European and North American participants representing 10.6%, 6.5% and 82.9% of tests, respectively. When restricted to US in-country tests, the annualized rate was 2.18 million, with four of 20 participants testing 79.2%. Among 73 respondents, 63 (86%) were for-profit, eight (11%) were non-profit academic or government supported and the remaining two included hospital-based and private non-profit. Eighteen (25%) supported relevant academic training. In 2011, screening for common trisomies was based on serum/ultrasound markers with an estimated 2.96 million US pregnancies screened in 131 laboratories. In 2022, cfDNA-based screening was offered by 20 laboratories testing 2.18 million US pregnancies.

Rapid Measurement of Total Saponins, Mannitol, and Naringenin in Dendrobium officinale by Near-Infrared Spectroscopy and Chemometrics

Dendrobium officinale has drawn increasing attention as a dual-use plant with herbal medicine and food applications. The efficient quality evaluation of D. officinale is essential to ensuring its nutritional and pharmaceutical value. Given that traditional analytical methods are generally time-consuming, expensive, and laborious, this study developed a rapid and efficient approach to assess the quality of D. officinale from different geographical origins by near-infrared (NIR) spectroscopy and chemometrics. Total saponins, mannitol, and naringenin were utilized as quality indicators. Two wavelength selection methods, namely, uninformative variable elimination and competitive adaptive reweighted sampling (CARS), were utilized to enhance the prediction accuracy of the quantification model. Moreover, multiple spectral pretreatment methods were applied for model optimization. Results indicated that the partial least squares (PLS) model constructed based on the wavelengths selected by CARS exhibited superior performance in predicting the contents of the quality indicators. The coefficient of determination (RP2) and root mean square error (RMSEP) in the independent test sets were 0.8949 and 0.1250 g kg−1 for total saponins, 0.9664 and 0.2192 g kg−1 for mannitol, and 0.8570 and 0.003159 g kg−1 for naringenin, respectively. This study revealed that NIR spectroscopy and the CARS-PLS model could be used as a rapid and accurate technique to evaluate the quality of D. officinale.

Evaluation of protein quality of wheat-rye flour blends by use of two small-scale analytical methods

Evaluation of protein quality of wheat-rye flour blends by use of two small-scale analytical methods

Verification report: Egalitarianism in young children

AbstractThe present study sought to evaluate the reproducibility of prominent findings stated by Fehr et al. in their developmental resource allocation experiment "Egalitarianism in Young Children", published in 2008. The experiment involved children making decisions about distributing sweets between themselves and either an in‐group or an out‐group recipient. Fehr et al. found that (1) inequity aversion develops with age; (2) 3‐ to 4‐year‐old children are inclined toward self‐advantageous allocations, whereas 7‐ to 8‐year‐olds distribute sweets more evenly in divisions, and (3) the influence of group status increases as children age. The original article stated that 229 Swiss school students aged 3 to 8 years (102 boys, 127 girls) participated in the study. However, no further demographics were reported. In our attempts to reproduce Fehr et al.'s original analyses and reanalyse the raw dataset, we found that one of the key variables was miscoded. After rectifying the miscoded variable, the reproduction results revealed only one ambiguously irreproducible result regarding a group status main effect in the sharing mini‐game—with three other tests exhibiting either strong reproducibility or ambiguous reproducibility. Reanalysis results indicated that Fehr et al.'s conclusions are robust when tested with alternative analytical tests.Highlights We evaluated the reproducibility of Fehr et al.'s (2008) highly cited developmental resource allocation findings. After identifying an inversely coded variable, we found all tests—bar one probit regression not related to major findings—to be reproducible. Reanalysis confirmed the robustness of Fehr et al.'s conclusions when using alternate analytical methods. Fehr et al.'s developmental resource allocation findings are reproducible and have theoretical implications for understanding inequity aversion and group status effects on resource allocation decisions in young children.

Interaction of Threonine with Biometal Chlorides in an Aqueous Environment at 25°C

The method for the synthesis of complexes with transition group biometal salts with the amino acid threonine includes improvement of reaction conditions, selection of reagents and analytical methods to confirm the formation of complexes. Research purpose: obtaining complex compounds of biometals, cobalt chloride, nickel chloride and manganese chloride with the amino acid threonine, as well as the study of their physicochemical and biological properties. In the synthesis of complex compounds, the preparative method was used. Compositions of the formed crystals were analyzed by IR spectroscopy. The structure and shape of cobalt, nickel and manganese crystals were determined using a microscope. The identity of the obtained compounds was confirmed by IR spectroscopy and microscopic analyses. We can conclude that threonine in the complex is coordinated to metal ions through the oxygen atoms of the carboxyl and nitrogen groups of the amine groups.

Bone-artefact production in late Neolithic central China: evidence from Pingliangtai

As an important component of prehistoric subsistence, an understanding of bone-working is essential for interpreting the evolution of early complex societies, yet worked bones are rarely systematically collected in China. Here, the authors apply multiple analytical methods to worked bones from the Longshan site of Pingliangtai, in central China, showing that Neolithic bone-working in this area, with cervid as the main raw material, was mature but localised, household-based and self-sufficient. The introduction of cattle in the Late Neolithic precipitated a shift in bone-working traditions but it was only later, in the Bronze Age, that cattle bones were utilised in a specialised fashion and dedicated bone-working industries emerged in urban centres.

Regression analysis for the determination of microplastics in sediments using differential scanning calorimetry.

This research addresses the growing need for fast and cost-efficient methods for microplastic (MP) analysis. We present a thermo-analytical method that enables the identification and quantification of different polymer types in sediment and sand composite samples based on their phase transition behavior. Differential scanning calorimetry (DSC) was performed, and the results were evaluated by using different regression models. The melting and crystallization enthalpies or the change in heat capacity at the glass transition point were measured as regression analysis data. Ten milligrams of sea sand was spiked with 0.05 to 1.5mg of microplastic particles (size: 100 to 200µm) of the semi-crystalline polymers LD-PE, HD-PE, PP, PA6, and PET, and the amorphous polymers PS and PVC. The results showed that a two-factorial regression enabled the unambiguous identification and robust quantification of different polymer types. The limits of quantification were 0.13 to 0.33mg and 0.40 to 1.84mg per measurement for semi-crystalline and amorphous polymers, respectively. Moreover, DSC is robust with regard to natural organic matrices and allows the fast and non-destructive analysis of microplastic within the analytical limits. Hence, DSC could expand the range of analytical methods for microplastics and compete with perturbation-prone chemical analyses such as thermal extraction-desorption gas chromatography-mass spectrometry or spectroscopic methods. Further work should focus on potential changes in phase transition behavior in more complex matrices and the application of DSC for MP analysis in environmental samples.