Standard Calibration Research Articles

Rapid and green quantification of phloridzin and trilobatin in Lithocarpus litseifolius (Hance) Chun (sweet tea) using an online pressurized liquid extraction high-performance liquid chromatography at equal absorption wavelength method.

Sweet tea is a functional herbal tea with anti-inflammatory, anti-diabetic, and other effects, in which phloridzin and trilobatin are two functional compounds. However, the current methods for their quantification are time-consuming, costly, and environmentally unfriendly. In this paper, we propose a rapid method that integrates online pressurized liquid extraction and high-performance liquid chromatography featuring a superficially porous column for fast separation. Moreover, we employ an equal absorption wavelength method to eliminate using multiple standard solutions and relative calibration factors. Our verification process corroborated the technique's selectivity, accuracy, precision, linearity, and detection limitations. Separately, our methodology demonstrated excellent analytical efficiency, cost-effectiveness, and environmental friendliness. Practical application using six distinct batches of sweet tea samples yielded results in congruence with the external standard method. The analytical rate of this technique is up to over 18 times faster than traditional methods, and organic solvent consumption has been reduced to less than 1.5 mL. Therefore, this method provides a valuable way to achieve quality control and green analysis of sweet tea and other herbal teas.

Determination of 145 pharmaceuticals and personal care products in eleven categories in water by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants frequently detected in aquatic environments at trace levels. These chemicals have diverse structures and physicochemical properties and includes pharmaceuticals like antibiotics, antihypertensive drugs, antiviral drugs, and psychotropic drugs that are widely used in large quantities worldwide. Considering the large number of pharmaceuticals currently in usage, it is crucial to establish a priority list of PPCPs that should be monitored and/or treated first. An accurate understanding of the occurrence and levels of PPCPs in aquatic environments is essential for providing objective materials for monitoring these emerging contaminants. Therefore, accurate, efficient, sensitive, and high-throughput screening techniques need to be established for determining and quantifying PPCPs. This study developed a method for the determination of 145 PPCPs (grouped into eleven categories: antibiotics, antihypertensive drugs, antidiabetic drugs, antiviral drugs, β-receptor agonists, nitroimidazoles, H2 receptor antagonists, psychotropic drugs, hypolipidemic drugs, non-steroidal anti-inflammatory drugs, and others) in water. The method was based on large volume direct injection without sample enrichment and cleanup and used ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS). Water samples were collected and filtered through a 0.22-μm regenerated cellulose (RC) filter membrane. Subsequently, Na2EDTA was added to the samples to adjust their pH to 6.0-8.0. Internal standards were mixed with the solutions, and because of the addition of Na2EDTA, the interference of metal ions could be eliminated in the determination of compounds, especially for tetracycline and quinolone antibiotics. Among the six filter membranes tested in this study (PES, PFTE-Q, PFTE, MCE, GHP, and RC), RC filter membranes were screened for water sample filtration. The UHPLC-MS/MS parameters were optimized by comparing the results of various mobile phases, as well as by establishing the best instrumental conditions. The 145 PPCPs were separated using an Phenomenex Kinetex C18 column (50 mm×3 mm, 2.6 μm) via gradient elution. The mobile phases were 0.1% (v/v) formic acid aqueous solution containing 5 mmol/L ammonium formate and acetonitrile for positive ion modes, 5 mmol/L aqueous solutions of ammonium formate and acetonitrile for negative ion modes. The samples were quantified using the scheduled multiple reaction monitoring (scheduled-MRM) mode with electrospray ionization in positive and negative ion modes. A standard internal calibration procedure was used to calculate contents of sample. The established method was systematically verified, and it demonstrated a good linear relationship. The average recoveries of the 145 PPCPs at the three spiked levels were in the range of 80.4%-128% with relative standard deviations (RSDs, n=6) of 0.6%-15.6%. The method detection limits (MDLs) ranged from 0.015 to 5.515 ng/L. Finally, the optimization method was applied to analyze the 145 PPCPs in 11 surface water samples and 6 drinking water samples. Overall, 93 (64%) out of the 145 analytes were detected. The total contents of the PPCPs in surface water samples ranged from 276.9 to 2705.7 ng/L. The detection frequencies of antidiabetic, antiviral, and psychotropic drugs were 100%. The total contents of the PPCPs in drinking water samples ranged from 140.5 to 211.5 ng/L, and antibiotics, antidiabetic drugs, and antiviral drugs comprised the largest proportion of analytes (by mass concentration) in drinking water samples. Our method exhibited high analytical speed and high sensitivity. It is thus suitable for the trace analysis and determination of the 145 PPCPs in environmental water and showed improved detection efficiency for PPCPs in water, indicating that it has a high potential for practical applications. This study can extend technical support for further pollution-level analysis of PPCPs in water and provide an objective basis for environmental management.

The development and validation of a new method for the fast determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn in rice by inductively coupled plasma optical emission spectrometry.

An alternative method of rice sample preparation for measuring the total content of selected elements, i.e., Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn, by ICP OES was developed. The proposed approach is based on the ultrasound-assisted extraction (USAE) of rice samples in the presence of a small amount of concentrated HNO3. The optimal operating parameters were found using the design of experiments (DOE) approach, and the studied experimental factors were the temperature of the ultrasonic bath (A), the sonication time (B), and the volume of concentrated HNO3 added per 0.5 g of a rice sample (C). Under the optimal conditions of the USAE procedure, i.e., A = 60 °C, B = 16 min and C = 4.0 mL, the rice samples were readily solubilized, and the obtained sample solutions could be analyzed by ICP OES with the simple standard solution calibration (without matrix matching). The analysis of the certified reference material (rice flour, NIST SRM 1568b) confirmed the satisfactory trueness of the USAE-ICP OES method. Additionally, no statistically significant differences between the results obtained for the samples prepared by USAE and open-vessel wet digestion (WD, the reference method) were found. In comparison to the routinely used microwave-assisted digestion and open-vessel digestion, the USAE approach offers lower acid consumption, lower detection limits (LODs) of elements, ranging from 4.0 ng g-1 for Mn to 2.7 µg g-1 for K, and a much shorter time of sample preparation.

Navigating Lp(a) Measurement Challenges: From Guidelines to Laboratory Perspectives

This comprehensive review delves into the evolving landscape of Lp(a) measurement standardsand examines the discordance and challenges in cardiovascular risk assessment in the contextof Lp(a). Acknowledging the shifting trends towards universal screening for Lp(a) endorsed by international societies working on risk assessment, management, and prevention of cardiovascular diseases, this review highlights the divergence in recommendations and the lackof consensus on Lp(a) risk thresholds. Ethnic variations in Lp(a) levels and ongoing clinical trial stargeting Lp(a) underscore the urgency of a unified and standardized approach to Lp(a) measurement. This article explores the intricacies of Lp(a) isoform size heterogeneity, availablemeasurement approaches, and the reporting unit challenge for the molecule. Emphasis is placed on collaborative efforts, transparent calibration, and the pivotal role of laboratories in ensuring the precision and reliability of Lp(a) measurements. The discussion encompasses thecall for unified calibration standards, highlighting the need for continuous external quality assessment and transparent reporting in clinical laboratories until a standardized Lp(a) measurement system is established.

A Fast-Forward Dilute-and-Shoot Multielement Method for Analysis of 33 Elements in Human Whole Blood, Serum, and Urine by Inductively Coupled Plasma Mass Spectrometry: A Streamlined Approach for Clinical Diagnostic and Biomonitoring.

The analysis of toxic and essential elements in human matrices is used in clinical diagnostics and for biomonitoring of different populations to study related health outcomes. This work aimed to develop fast and reliable methods for the analysis of a broad range of elements in liquid human matrices, such as whole blood, serum, and urine, with a similar setup for the three matrices and different analysis needs. An easy and fast-forward dilute-and-shoot method for 33 elements (i.e., Ag, Al, As, B, Ba, Be, Bi, Cd, Ce, Co, Cr, Cu, Hg, I, Li, Mn, Mo, Ni, Pb, Pd, Pt, Sb, Se, Sn, Sr, Te, Th, Tl, U, V, W, Zn, and Zr) was developed. 200 µL of either sample material was diluted with an alkaline reagent to a volume of 4 mL in total. Sample dilution and preparation of matrix-matched calibration standards were performed in 48-well plates by an automated liquid handler. Diluted samples were analyzed by inductively coupled plasma mass spectrometry on a Perkin Elmer NexIon 300D ICP-MS instrument equipped with an ESI-FAST SC2DX autosampler in kinetic energy discrimination mode with helium as cell gas at either 4.8 mL or 5.7 mL and 1600 W RF generator power. The method validation results showed good accuracy for fresh human samples from an external quality assessment scheme with measured concentrations within the assigned concentration ranges. Good precision and reproducibility for most elements were demonstrated with variation coefficients below or far below 8% and 15% for whole blood, 8% and 10% for serum, and 10% and 10% for urine, respectively. The developed reagent and instrumental setup were applicable to all three matrices. This minimizes the risk of human errors when switching between analyses of the different sample matrices and allows a rapid and easy analysis of whole blood, serum, and urine within one day if needed. The method demonstrated robustness over time, withstanding minor changes in the preparation of working solutions and samples, instrumental analysis, and setup. Analysis of human real samples showed the method's applicability for 33 toxic and essential elements in whole blood, serum, and urine and at concentrations relevant to clinical diagnostics as well as biomonitoring.

Development and validation of an LC-MS/MS method for ruxolitinib quantification: advancing personalized therapy in hematologic malignancies.

Hematologic malignancies such as leukemia and lymphoma present treatment challenges due to their genetic and molecular heterogeneity. Ruxolitinib, a Janus kinase (JAK) inhibitor, has demonstrated efficacy in managing these cancers. However, optimal therapeutic outcomes are contingent upon maintaining drug levels within a therapeutic window, highlighting the necessity for precise drug monitoring. We developed a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify ruxolitinib in human plasma, improving upon traditional methods in specificity, sensitivity, and efficiency. The process involved the use of advanced chromatographic techniques and robust mass spectrometric conditions to ensure high accuracy and minimal matrix effects. The study was conducted using samples from 20 patients undergoing treatment, with calibration standards ranging from 10 to 2000ng/mL. The method displayed linearity (R 2 > 0.99) across the studied range and proved highly selective with no significant interference observed. The method's precision and accuracy met FDA guidelines, with recovery rates consistently exceeding 85%. Clinical application demonstrated significant variability in ruxolitinib plasma levels among patients, reinforcing the need for individualized dosing schedules. The validated LC-MS/MS method offers a reliable and efficient tool for the therapeutic drug monitoring of ruxolitinib, facilitating personalized treatment approaches in hematologic malignancies. This approach promises to enhance patient outcomes by optimizing dosing to reduce toxicity and improve efficacy.

Calibration-free reaction yield quantification by HPLC with a machine-learning model of extinction coefficients.

Reaction optimization and characterization depend on reliable measures of reaction yield, often measured by high-performance liquid chromatography (HPLC). Peak areas in HPLC chromatograms are correlated to analyte concentrations by way of calibration standards, typically pure samples of known concentration. Preparing the pure material required for calibration runs can be tedious for low-yielding reactions and technically challenging at small reaction scales. Herein, we present a method to quantify the yield of reactions by HPLC without needing to isolate the product(s) by combining a machine learning model for molar extinction coefficient estimation, and both UV-vis absorption and mass spectra. We demonstrate the method for a variety of reactions important in medicinal and process chemistry, including amide couplings, palladium catalyzed cross-couplings, nucleophilic aromatic substitutions, aminations, and heterocycle syntheses. The reactions were all performed using an automated synthesis and isolation platform. Calibration-free methods such as the presented approach are necessary for such automated platforms to be able to discover, characterize, and optimize reactions automatically.

Rapid determination of 87 prohibited ingredients in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

The methods of detecting numerous prohibited components are not included in the Technical Specifications for Cosmetic Safety (2015 Edition). Recently, owing to its high speed, sensitivity, and anti-interference properties, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) became the preferred method of detecting banned substances in cosmetics. In this study, a UPLC-MS/MS method was developed for use in determining 87 prohibited ingredients in cosmetics, including 33 sex hormones, 20 anti-infective drugs, 15 antihistamines, 7 coumarins, 4 sedative-hypnotic drugs, 4 antipyretic and analgesic drugs, 2 allergenic fragrances, and 2 drugs with vasoconstriction effects. The main factors affecting the response, recovery, and sensitivity of the method, such as the type of extraction solvent, extraction time, ratio of the mobile phases, and MS conditions, were optimized during sample pretreatment and instrumental analysis. Accordingly, approximately 0.2 g of the toner or cream sample was dispersed in 2 mL acetonitrile in a 10 mL colorimetric tube. After diluting to 10 mL with 50% acetonitrile aqueous solution, the sample was ultrasonically extracted for 20 min and centrifuged, and the mixture was then filtered through a 0.22 μm membrane. Approximately 0.2 g of the oil sample was dispersed in 2 mL n-hexane in a 15 mL polypropylene centrifuge tube and extracted twice with 3 mL 70% acetonitrile aqueous solution. The extracts were transferred into a 10 mL colorimetric tube and diluted to 10 mL with 50% acetonitrile aqueous solution, and the mixture was then filtered through a 0.22 μm membrane. The samples were separated using a CORTECS C18 column (150 mm×2.1 mm, 2.7 μm), employing a gradient elution program with acetonitrile and 0.1% formic acid aqueous solution as the mobile phases. The flow rate, column temperature, and injection volume were respectively set at 0.3 mL/min, 40 ℃, and 2 μL. The 87 compounds were monitored in multiple reaction monitoring (MRM) mode with electrospray ionization (ESI) under positive and negative conditions. Matrix-matched external standard calibration was used for quantification, and the analysis was completed within 33 min. The prohibited compounds exhibited good linear relationships, with r values of >0.99, and the limits of detection (LODs) and quantification (LOQs) for the 87 compounds were 0.07-0.38 and 0.21-1.15 μg/g, respectively. Three types of cosmetic matrices were selected to verify the recovery and precision of the method at LOQ, 2 LOQ, and 10 LOQ levels. The average recoveries of the 87 prohibited compounds were in the range of 81.7%-115.4%, and the relative standard deviations (RSDs, n=6) were 0.4%-9.9%. The reliability of the developed method was demonstrated by applying it to 349 commercial cosmetics obtained from the market, and 8 positive samples were identified. The positive components included trimethoprim, terbinafine, naphazoline, 7-methoxycoumarin, and 7-methylcoumarin. The established method displays the advantages of simple operation and rapidness and a high sensitivity and good recovery. And, this method provides technical support for rapid risk screening and the revision of national standards for cosmetics.

External standard calibration method for high-repetition-rate shock tube kinetic studies with synchrotron-based time-of-flight mass spectrometry.

The signal levels observed from mass spectrometers coupled by molecular beam sampling to shock tubes are impacted by dynamic pressures in the spectrometer due to rapid pressure changes in the shock tube. Accounting for the impact of the pressure changes is essential if absolute concentrations of species are to be measured. Obtaining such a correction for spectrometers operated with vacuum ultra violet photoionization has been challenging. We present here a new external calibration method which uses VUV-photoionization of CO2 to develop time-dependent corrections to species concentration/time profiles from which kinetic data can be extracted. The experiments were performed with the ICARE-HRRST (high repetition rate shock tube) at the DESIRS beamline of synchrotron SOLEIL. The calibration experiments were performed at temperatures and pressures behind reflected shock waves of 1376 ± 12 K and 6.6 ± 0.1 bar, respectively. Pyrolytic experiments with two aromatic species, toluene (T5 = 1362 ± 22 K, P5 = 6.6 ± 0.2 bar) and ethylbenzene (T5 = 1327 ± 18 K, P5 = 6.7 ± 0.2 bar), are analyzed to test the method. Time dependent concentrations for molecular and radical species were corrected with the new method. The resulting signals were compared with chemical kinetic simulations using a recent mechanism for pyrolytic formation of polycyclic aromatic hydrocarbons. Excellent agreement was obtained between the experimental data and simulations, without adjustment of the model, demonstrating the validity of the external calibration method.

Application of the QuEChERS method combined with UHPLC-QqQ-MS/MS for the determination of isoprocarb and carbaryl pesticides in Indonesian coffee.

The performance of the QuEChERS method in this study, as indicated by a high percentage (>90%) of recovery observations falling within the range of 60-140% and a sample replicate deviation (% RSD) of <20%, for the routine analysis of isoprocarb and carbaryl pesticides, has been evaluated over a 14-month period for the export of Indonesian coffee. Following a seven-day observation of the stability of these pesticides in coffee extract, it was found that the added standard calibration solution remained stable and useable for seven days when stored at 4 °C and -20 °C. This validated method, with high sensitivity (a LOQ of 0.001 mg kg-1 for isoprocarb and carbaryl), has been employed to monitor residues in Indonesian coffee exports to comply with maximum residue limits (MRLs). The samples with higher contamination levels were predominantly from robusta coffee (57.76%), followed by arabica coffee (6.17%). The detection rates for residues decreased by more than 90% in the last two months of the method's application. In the observation of coffee processing, it was found that isoprocarb residues in contaminated samples could be transferred to the processed coffee (roasted and its infusion) to a limited extent, while residues from the carcinogenic carbaryl were not detected due to evaporation. Additionally, chronic dietary risk assessment showed that contaminated samples of robusta and arabica coffees should not be considered a significant public health concern (hazard index HI < 1). However, continuous monitoring of pesticide residues in Indonesian coffee is still recommended, not only to conform to the MRLs of importing countries but also to ensure food trade.

Determination of tetrodotoxin in urine by liquid chromatography-tandem mass spectrometry with internal standard calibration

An analytical method was developed for tetrodotoxin(TTX) in urine by liquid chromatography-tandem mass spectrometry(LC-MS/MS) with internal standard calibration. TTX in the sample was extracted with the mixture of acetic acid/methanol/acetonitrile(0.005 mL/0.8 mL/1.8 mL), cleaned by solid phase extraction(SPE) with cation exchange cartridge, eluted with 50% acetonitrile/water containing 0.3% hydrochloric acid, and neutralized with ammonia. The extract was separated by a Waters XBridge~(TM) BEH Amide column(150 mm×3.0mm, 1.7 μm) and measured by MS/MS. By optimizing sample extraction and SPE cleanup conditions, the problems of low recovery and strong suppression effects of MS signal for TTX in urine were resolved when cleaned with cation exchange cartridge. Quantitatively calibrated by the internal standard of Kasugamycin, good linear relationship was found for TTX in urine at the range of 0.2-200 μg/L with the correlation coefficient(r~2) of 0.997. The limits of detection and quantitation for TTX in sample matrix were 0.1 and 0.2μg/L, respectively. The average recoveries at three spiking levels(0.2, 10.0 and 200 μg/L) were 89.3%-95.3% with relative standard deviation(n=6) less than 5.1%. The concentrations of TTX in urine from 11 poisoning patients were 0.4-138 μg/L. The detection rate was 100% in urine collected within 3 days after poisoning. The established method was simple, accurate and sensitive. It can provide reliable technical support for the rapid treatment of TTX poisoning events and the study of toxin metabolism in vivo.

A standard calibration method based on a symmetric resistance network matrix for galvanic logging instruments.

An increasing number of measurement electrodes have been designed to satisfy the demand for high-resolution detection using galvanic logging technology in complex formations. The forward modeling response analysis of logging tools has important guiding significance in the design of galvanic logging tools. Based on a three-dimensional finite element numerical simulation method, we established a forward model of galvanic multi-electrodes in a complex formation. We also designed a symmetrical resistance network model of the formation with equivalent resistance between two electrodes. A symmetrical resistance network was derived using the balanced bridge method. The asymmetrical admittance matrix was extended to a symmetrical extended admittance matrix to realize a convenient calculation of the equivalent symmetrical resistance network in complex formations. Verification of the microcolumn-focused logging tool, with nine electrodes in a simulated standard well, and an evaluation of the degree of invasion in an actual oil well indicate that this calibration method can improve the measurement accuracy of galvanic logging instruments.

Direct determination of lithium in brine samples using handheld LIBS without sample treatment: sample introduction by venturi system.

Splashing is the main problem for the direct analysis of aqueous samples using LIBS since it generates serious precision and accuracy issues. This study demonstrates the direct determination of Li content in brines for the control of industrial mining processes using a portable LIBS device based on the direct laser impact on the sample, without any sample treatment, through the design of a sample injection system based on the Venturi effect. Our results demonstrated that the utilization of the 653.3 nm hydrogen line as an internal standard reduces the model calibration fitting error from 0.440 root mean square error in a standard calibration curve to 0.123 on the internal standard curve. Conversely, the development of a Venturi effect-based injection device using compressed air converts the brine into a fine mist which decrease splashing, resulting in an up to 10-fold error reduction, all without the necessity of employing an internal standard. Our results, evaluated by comparing them to the ASTM D3561-11 standard method using flame atomic absorption spectrometry, indicate that it is feasible to determine the lithium content in brine samples with an error of under 20% and a detection limit of 13 mg kg-1.

Enhancing Bone Infection Diagnosis with Raman Handheld Spectroscopy: Pathogen Discrimination and Diagnostic Potential.

Osteomyelitis is a bone disease caused by bacteria that can damage bone. Raman handheld spectroscopy has emerged as a promising diagnostic tool for detecting bone infection and can be used intraoperatively during surgical procedures. This study involved 120 bone samples from 40 patients, with 80 samples infected with either Staphylococcus aureus or Staphylococcus epidermidis. Raman handheld spectroscopy demonstrated successful differentiation between healthy and infected bone samples and between the two types of bacterial pathogens. Raman handheld spectroscopy appears to be a promising diagnostic tool in bone infection and holds the potential to overcome many of the shortcomings of traditional diagnostic procedures. Further research, however, is required to confirm its diagnostic capabilities and consider other factors, such as the limit of pathogen detection and optimal calibration standards.

Color Standardization and Stain Intensity Calibration for Whole Slide Image-Based Immunohistochemistry Assessment.

Automated quantification of human epidermal growth factor receptor 2 (HER2) immunohistochemistry (IHC) using whole slide imaging (WSI) is expected to eliminate subjectivity in visual assessment. However, the color intensity in WSI varies depending on the staining process and scanner device. Such variations affect the image analysis results. This paper presents methods to diminish the influence of color variation produced in the staining process using a calibrator slide consisting of peptide-coated microbeads. The calibrator slide is stained along with tissue sample slides, and the 3,3'-diaminobenzidine (DAB) color intensities of the microbeads are used for calibrating the color variation of the sample slides. An off-the-shelf image analysis tool is employed for the automated assessment, in which cells are classified by the thresholds for the membrane staining. We have adopted two methods for calibrating the color variation based on the DAB color intensities obtained from the calibrator slide: (1) thresholds for classifying the DAB membranous intensity are adjusted, and (2) the color intensity of WSI is corrected. In the experiment, the calibrator slides and tissue of breast cancer slides were stained together on different days and used to test our protocol. With the proposed protocol, the discordance in the HER2 evaluation was reduced to one slide out of 120 slides.

Surface breaking crack sizing method using pulse-echo Rayleigh waves

Surface cracks are common in various industries. Eddy current testing (ECT) is commonly used for crack sizing but necessitates complex calibration standards and a highly trained inspector. Moreover, for large-area inspections, it requires additional scanning arrangements. In recent years the wedge technique-based Rayleigh wave crack sizing method has attracted significant research interest due to its unidirectional excitability. However, Rayleigh wave features generated at crack tips are often weak and masked under noise, and they mostly attenuate before reaching the receiving probe due to the couplant between the wedge-test specimen interface. Consequently, sizing the crack depth is difficult using a pulse-echo setup. This work presents a wedge-free pulse-echo Rayleigh wave method for surface crack sizing using a conventional phased array transducer. Eliminating the wedge removes a couplant layer leading to lower attenuation, enabling the transducer to capture crack tip features. This allows the sizing of surface cracks in pulse-echo using the time-of-flight (ToF) information. Furthermore, leveraging the phased array system, an averaging technique employed to the time trace signals captured by the transducer elements effectively averages out the other wave modes generated at crack geometries by the scattering of Rayleigh waves. This significantly minimizes sizing errors and enhances the signal-to-noise ratio (SNR). The performance of the proposed method is demonstrated through finite element simulations and experiments. Experiments with electric discharged machined (EDM) notches on test specimen surface at various angles and depths mimicking surface-breaking cracks show accurate sizing within a 5% error. The proposed method offers flexibility in performing inspections using a wide frequency range and can be easily applied to different materials using any conventional phased array transducer. This enhances its adaptability for industrial applications in the characterization of surface cracks.

Fraunhofer line-based wavelength-calibration method without calibration targets for planetary lander instruments

High-accuracy wavelength calibration is critical for qualitative and quantitative spectroscopic measurements. Many spectrometers employed in planetary-exploration missions have onboard calibration sources, including standard lamps and calibration targets. However, such calibration sources are not always available because planetary missions, particularly landing missions, usually have limitations in size and mass. Thus, a wavelength calibration method without requiring hardware addition can be highly beneficial. In this study, we demonstrate a method for wavelength calibration using solar Fraunhofer lines observed in the reflectance spectra of planetary surfaces. Using a Raman spectrometer prototype developed for a Phobos rover, we measured the spectrum of the sunlight reflected from a spectral standard, manufactured to provide similar reflectance spectra to the surface of Phobos. We identified 35 Fraunhofer absorption lines in the wavelength range between 530 and 700 nm and utilized these features for the wavelength calibration of the spectrometer. This approach using Fraunhofer lines achieved good results (better than +0.04/−0.06 nm), comparable to the results achieved using a conventional Ne lamp. The wavelength accuracy corresponds to a wavenumber accuracy better than ±1.5 cm−1 in the 0–4000 cm−1 Raman shift (Stokes shift) range with a 532 nm excitation laser. This result enabled the estimation of the magnesium number (Mg#) of olivine, achieving a value more precise than 1.5% based on the Raman peak positions. In addition, we examined the number of solar Fraunhofer lines detectable at different wavelength resolutions by binning the solar spectrum acquired in this study. We found that more than 10 Fraunhofer lines could be detected as prominent absorption lines when the wavelength resolution is higher than 1 nm/pix (30 cm−1/pix at 1000 cm−1). This result suggests that the target-free wavelength-calibration method using solar Fraunhofer lines can be applied to other spectrometers simply by observing sunlit planetary surfaces.

Does radiographic calibration affect linear radiographic measurements in a large pediatric spine registry?

Large registries are increasingly at the forefront of modern pediatric spine research, with manual, centralized, trained radiographic measurement serving as the gold standard for spine research. However, there is limited data regarding the reliability of registry measurements which may be subject to differences in radiographic calibration.We undertook this study to evaluate reliability of T1-T12 height, L1-S1 height, and coronal balance measurements for a large registry of early onset scoliosis patients. Three trained technicians from the Pediatric Spine Study Group measured 43 radiographs for T1-T12, L1-S1, and coronal balance using 3 different calibration techniques. All radiographs were AP views of patients with magnetically controlled growing rods with known diameters. The calibration techniques used a pre-export manually drawn line, a digital automatically generated computerized marker, and the diameter of a magnetically controlled growing rod.The intraclass correlation coefficient (ICC) was calculated to determine reliability. 1161 measurements were performed.For each of the three raters, coronal balance, T1-T12 height and L1-S1 height had excellent agreement regardless of the calibration technique (alpha 0.93-1.0).Among the parameters, coronal balance had the worst inter-rater reliability, whereas there was excellent interrater reliability regarding T1-T12 height and L1-S1 height (alpha 0.91-0.99). There was excellent agreement among reviewers and between the 3 different calibration techniques. While calibration using rod diameter served as the gold standard, this data shows that other standard calibration methods were adequate and achieved excellent reliability for registry radiographs.

Solubility and Taste Masked Behaviour of Cyclodextrin Molecular Inclusion Complex of Artemether

Artemether by forming a complex with β-cyclodextrine (βCD) is used to improve solubility and taste masked by the kneading method. Artemether with β-cyclodextrine complex prepared with βCD in a drug-polymer ratio 1:1 gave complete taste masking with the satisfactory result obtained in term of in-vivo and in-vitro evaluation. The standard calibration curve of Artemether shows a slope of 0.0154 and a correlation coefficient of 0.9992. Compatibility studies show that drugs are compatible with polymers. Solubility studies show that the solubility of drug are increased in Phosphate buffer 6.8 by successfully forming a complex with βCD. In-vitro dissolution results showed that a maximum of 97.05% of Artemether, drug release less than 15 minutes in formulation. The solubility of Artemether in saliva (PH 6.8) is 0.00735 mg/mL, After complex forming with β-cyclodextrin the solubility of (Artemether complex) is 0.124 mg/mL. In-vitro drug release investigation, taste masking occurs when the amount of drug substance in the dissolve medium is either not identified or is below the threshold for recognizing its flavor in the early time points (between 0 and 5 minutes). Taste masking ( Taste perception test) 11 volunteers were selected for this test, results show that complex is taste masked. Artemether with βCD complex is a hopeful method to augment the solubility, dissolution and taste masking of the drug.

Solubility and Taste Masked Behaviour of Cyclodextrin Molecular Inclusion Complex of Lumefantrin

Lumefantrine is an antimalarial drugs used especially for pediatric persons. β-Cyclodextrine is used to improve the taste of lumefantrine by forming complexes with them by the solvent evaporation method, respectively. β-Cyclodextrine prevent the release of drug in the saliva. Lumefantrine is a bitter drug. So masking of bitter taste in the formulation is a prerequisite as it improves the compliance of the patient and product value. Lumefantrine with β-cyclodextrin in a drug-polymer ratio 1:1 gave complete taste masking with a satisfactory result obtained in term of in-vivo and in-vitro evaluation visual inspection revealed that lumefantrine was yellow-crystalline. The melting point of lumefantrine was found to be 127℃, respectively. The standard calibration curve of Lumefantrine shows a slope 0.0108 and a correlation coefficient of 0.9997. Compatibility studies show that drugs are compatible with polymers. Solubility study show that the solubility of both drugs are increased in phosphate buffer 6.8 by successfully forming a complex with β-cyclodextrin. The solubility of lumefantrine in saliva (pH 6.8) is 0.408 mg/mL, after complex forming with β-cyclodextrine the solubility of (Lumefantrine complex) is 0.526 mg/mL. In an in-vitro drug release investigation, taste masking occurs when the amount of drug substance in dissolved media is either below the detection threshold for recognizing its taste or is undetectable in the early time points (between 0 and 5 minutes). Taste masking (Taste perception test) 11 volunteers are selected for this test, results show that complex is taste masked successfully. Lumefantrine with β-Cyclodextrine complex is a hopeful approach to enhance solubility, dissolution and drug taste.