Determination of 99Tc in TBP phase in spent nuclear fuel reprocessing with plastic scintillation resin.

Objective: The objective is described to develop and validate a simple, reliable, precise, and specific analytical method for rapid separation and determination of N-oxide impurity in rizatriptan Benzoate active pharmaceutical ingredient bulk drug substances by reverse phase liquid chromatography as per the International Conference on Harmonization (ICH) guidelines.Methods: The methodology utilized as reverse phase liquid chromatography with gradient composition. The mobile phase proportion was compromised mobile A containing 0.25 mm potassium dihydrogen phosphate buffer pH 2.0 and methanol (95:5 v/v) and mobile B containing Acetonitrile. ODS 3V, 250 × 4.6 mm, 5 µm. column. The flow rate is 1.0 ml/minute using an LC system detector at wavelength 280 nm, and the column oven temperature is 40°C. The chromatographic separation performed in reverse phase by the gradient composer over run time was 35 minute. The resolution between N-oxide and rizatriptan was recorded on the chromatogram was more than six. The developed analytical method was validated according to the ICH guidelines.Results: Linearity was found in rizatriptan N-oxide over the concentration range of 450-11000 ng/ml, with the linear regression (Correlation coefficient R = 0.999) and proved to be robust. Limit of detection and limit of quantification of the rizatriptan N-oxide was found 150 and 450 ng/ml. The retention time of rizatriptan and rizatriptan N-oxide was recorded 22.6 and 24.7 minutes, respectively. The percentage recovery of N-oxide has been ranged from 96.0 to 102.0 in the bulk drug material sample. The proposed analytical method has been found suitable, precise, reliable, and accurate for the separation and quantitative determination.Conclusion: A specific, simple, accurate, reliable, and rapid reproducible analytical method has been developed and validated for reverse phase high- performance liquid chromatography to determine N-Oxide impurity in rizatriptan benzoate from bulk drugs material as per ICH guideline.Keywords: Rizatriptan benzoate, N-oxide impurity, High performance liquid chromatography, Reverse phase, ODS column and validation.

The presence of acrylamide, a known human carcinogen, in various heated foods raises significant concerns among consumers. Therefore, the development of a good analytical method is of paramount interest to the scientific community. Keeping this in view, a rapid, simple, reliable, and low-cost analytical method was developed and validated for acrylamide quantification in black ripe olives. The method consisted of the water extraction of the compounds from crushed olives with the addition of (13C3)acrylamide as an internal standard. The quantification was performed using high-pressure liquid chromatography and mass detection with positive electrospray ionization. The limits of detection and quantification were determined to be 4 and 11 µg/kg, respectively. The developed method exhibited excellent results in terms of accuracy (98.4–104.8%) and intra- and inter-day precision limits, both less than 20%. This new method was carried out by analyzing 15 samples of Spanish commercial black ripe olives, revealing a wide range of values, from 79 to 1068 µg/kg of fruit. The new protocol reduces the analysis time to just one hour per sample versus the minimum 24 h required by gas chromatography and mass detection, meaning that it could be a good option for the routine analysis of acrylamide in black ripe olives, and may be extendable to the analysis of this compound in other foods.

Objective: The objective of the this work is to develop and validate a novel, simple,rapid and reliable analytical method for separation and determination of R-isomer impurity in Etodolac bulk drug material by normal-phase high-performance liquid chromatography as per International Conference on Harmonization guidelines. Methods: The Etodolac R- isomer and S-isomer were separated on a Chiralcel OD-H (150 x 4.0 mm, 5 micron) column by using Ethanol : n-Hexane:Trifluoroacetic acid (50:50:0.1 v/v.) mobile phase with equipped detector at wavelength 225 nm and 25 °C column oven temperature. The resolution between R-isomer and S-isomer were more than two recorded on chromatogram. The specified method was developed and validated for various parameters like reproducibility, limit of detection, limit of quantification, linearity and range, robustness, solution stability and mobile phase stability according to the International Conference on Harmonization (ICH) guidelines. Results: Linearity were found for Etodolac R-isomer over the concentration range of 600–6000 ng/ml, with the linear regression (Correlation coefficient R = 0.998) and proved to be robust. Limit of detection and limit of quantification of Etodolac R-isomer was found to be 200 and 600 ng/ml. The retention time of R-isomer was considered to be 2.8 min. The percentage recovery of Etodolac R-isomer has been ranged from 97.0 to 102.0 in bulk drug material sample. The proposed analytical method has been found to be suitable, precise,reliable and accurate for the separation and quantitative determination of Etodolac R-isomer in bulk drug sample. Conclusion: A novel, speedy, accurate, precise, reliable and rugged analytical method has been developed and validated for normal phase high performance liquid chromatography to determine R-isomer impurity in Etodolac bulk drugs material as per ICH guideline. Keywords: Etodolac, HPLC, Known Impurity. Normal Phase, Validation.

A rapid and reliable solid-phase extraction method for HPLC analysis of opium alkaloids from Papaver plants was established. Fifty mg of dried and powdered plant sample was extracted with 5 ml of 5% acetic acid for 30 min under sonication. After centrifugation, 3 ml of the supernatant was loaded on a reversed-phase cation-exchange solid-phase extraction cartridge. After seriate washings with 0.1 M hydrochloric acid and methanol, alkaloids were eluted with a mixture of 28% ammonia and methanol (1:19). The eluate was concentrated under nitrogen stream at 40 degrees C and the residue was dissolved in 50% aqueous methanol for high performance liquid chromatographic analysis. With this solid-phase extraction method, the recovery of morphine, codeine, oripavine, thebaine, papaverine, noscapine and sanguinarine was from 99.94 to 112.18% when the standard alkaloids were added to the plant samples. Opium alkaloids of a variety of genus Papaver plants cultivated in a field and phytotron were analyzed by this method.

A rapid, environmentally friendly, and reliable method for pesticide analysis in high-fat samples

14C is one of the limiting radionuclides used in the categorization of radioactive graphite waste; this categorization is crucial in selecting the appropriate graphite treatment/disposal method. We propose a rapid analysis method for 14C specific activity determination in small graphite samples in the 1–100 μg range. The method applies an oxidation procedure to the sample, which extracts 14C from the different carbonaceous matrices in a controlled manner. Because this method enables fast online measurement and 14C specific activity evaluation, it can be especially useful for characterizing 14C in irradiated graphite when dismantling graphite moderator and reflector parts, or when sorting radioactive graphite waste from decommissioned nuclear power plants. The proposed rapid method is based on graphite combustion and the subsequent measurement of both CO2 and 14C, using a commercial elemental analyser and the semiconductor detector, respectively. The method was verified using the liquid scintillation counting (LSC) technique. The uncertainty of this rapid method is within the acceptable range for radioactive waste characterization purposes. The 14C specific activity determination procedure proposed in this study takes approximately ten minutes, comparing favorably to the more complicated and time consuming LSC method. This method can be potentially used to radiologically characterize radioactive waste or used in biomedical applications when dealing with the specific activity determination of 14C in the sample.

Soybean contains nutritional bioactive compounds, including carotenoids associated with human health benefits. Carotenoids are applicable in pharmaceuticals/nutreceuticals, cosmetic, and mainly food industries. However, an efficient and accurate method for carotenoid and chlorophyll detection and quantification has not yet been developed and validated for soybean seeds. The need for a rapid and reliable analysis method has become increasingly important. Thus, this study was initiated to develop and validate a simple, rapid, and selective reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of lutein, zeaxanthin, α-carotene, β–carotene, β–cryptoxanthin, and chlorophyll–a and –b in soybean flour sample (100.00 mg) extracted using ethanol-acetone (1:1) solvents at a volume of 1.50 mL. Interestingly, the effective separation technique was achieved using the mobile phases of methyl tert-butyl ether, methanol containing 10 mM ammonium acetate, and water delivered at a 0.90 mL min−1 flow rate through a C30YMC Carotenoid (250 × 4.6 mm I.D., S-5 µm) column coupled with a UV-VIS detector set at 450 nm. The detector response was linear from 0.05–30.00 μg mL−1 with a coefficient of determination (R2) of 0.9993–0.9999. The validated method was sensitive with a detection limit (LOD) of 0.0051–0.0300 μg mL−1 and 0.0155–0.0909 μg mL−1 for the quantification limit (LOQ). The recovery values were from 83.12–106.58%, and the repeatability precision ranged from 1.25–4.20% and 0.15–0.81% for the method and system, respectively. The method showed adequate precision with a relative standard deviation smaller than 3.00%. This method was also found to be applicable for profiling carotenoids and chlorophylls in other legumes. In summary, this method was successfully implemented for qualitative and quantitative determination of major carotenoids and chlorophylls in soybean and other legume seeds, which are beneficial to food industry and quality breeding programs to meet human nutrition demands globally.

Preservatives are frequently added to cosmetics to maintain product quality. Our laboratory quantifies 11 preservatives in cosmetics each year for regulatory purposes. In laboratories, many manufactures also analyze the preservatives in their products for quality control. To analyze many cosmetic samples, a rapid analysis method is required for efficiency. In this study, we developed a rapid method for the simultaneous determination of 11 regulated preservatives in cosmetics using a core-shell column by high-performance liquid chromatography. In this method, the 11 preservatives were separated within 17min, which was approximately half the time reported in the previous study. The peak resolution for each preservative was >2.6, the correlation coefficients of the calibration curves were >0.9988, the percent recoveries were 92.0-111.9% and the relative standard deviations were <3.5% (n = 3). The relative standard deviations among 6 researchers were <4.7%. Thus, it is an effective rapid determination method for the analysis of preservatives in cosmetics.

Nanocoating cellulose paper based microextraction combined with nanospray mass spectrometry for rapid and facile quantitation of ribonucleosides in human urine

A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

Mortality from plague is high if not treated with the proper antibiotics within 18-24 hours after onset of symptoms. The process of antibiotic susceptibility determination of Yersinia pestis isolated from blood samples may extend from 4 to more than 7 days, since the in vitro growth is very slow. To accelerate this process, we developed an enrichment protocol as well as a non-standard yet reliable method for rapid antibiotic susceptibility analysis of Y. pestis from blood cultures using flow cytometry technology. This rapid method is applicable to blood cultures containing low levels of Y. pestis.

A rapid, simple, sensitive and cost-effective analytical method has been standardised to determine the residues of imidacloprid and thiamethoxam in soil. This method does not require any cleanup with costly sorbents. The recoveries of imidacloprid and thiamethoxam obtained in this no-cleanup method were on par with the protocol involving primary–secondary amine-based cleanup. This method requires less volume of solvent (20 mL of acetonitrile/sample) and is suitable for high throughput analyses involving large number of samples. The limit of quantification of the method was 0.01 μg/g. Dissipation kinetics of imidacloprid and thiamethoxam in the soils of sugarcane ecosystem was studied by adopting this rapid method. The half-life of imidacloprid and thiamethoxam was 9.07 and 6.22 days when applied at 70 and 100 g a.i./ha, respectively. The dissipation of both the neonicotinoids followed first-order kinetics with good fit.

A rapid, sensitive and selective analytical method by LC-MS/MS was developed and validated for the determination of cyclamate in various kinds of foods. The Preparation of test solutions was performed by heat extraction technique in accordance with an official notification method in Japan. We aimed to reduce the matrix effects in LC-MS/MS only by diluting extracts without clean-up using solid phase column. This method was assessed for 30 kinds of foods fortifying cyclamate at the concentration level of 0.5 μg/g. As a result, trueness was 85.0 to 106.6%, repeatability (RSDr) ranged from 1.7 to 9.4%, and within-laboratory reproducibility (RSDwr) ranged from was 4.1 to 9.7%. These date supported the reliability our method. Thus, this method could be useful for a rapid determination of cyclamate in various kinds of foods.

In most soil testing laboratories, textural analysis is performed by the pipette method (PM) or by hydrometer. Objectives of this study were (i) to evaluate simplified methods that can be used for soils of various textures, and (ii) to modify a rapid method for reliable and accurate textural analysis of saline and alkaline soils. One hundred soils were collected from different agro‐ecological regions of India. Coefficients of variation for sand, silt, and clay of soil samples by the rapid method varied across a range of 0 to 5% with a mean value &lt;3% for all soils. Absolute differences between the PM and the rapid method for sand, silt, and clay fractions ranged from −1.8 to 1.7, −1.8 to 5.3, and −2.9 to 1.8%, with averages across the sites of −0.04, 2.92, and −6.52%, respectively. Among various methods, regression analysis between the rapid and pipette methods produced the highest coefficient of determination ( r 2 ) values of 0.9989, 0.9927, and 0.9930 for sand, silt, and clay fractions, respectively. A rapid method with modified sodium hexametaphosphate concentrations and soil shaking periods produced mean, standard error, and standard deviation values very close to the PM, with r 2 values &gt;0.99 with small intercepts &lt;0.5, &lt;0.3, and &lt;0.7 for saline, saline–alkaline, and alkaline soils, respectively. The rapid method with proposed modifications provides the most accurate and fast estimation of texture for saline–alkaline soils.

A rapid separation method was developed for determination of low level promethium-147 and samarium-151. The rapid method, applied to environmental samples, provided speed and efficiency for the respective separation of Pm and Sm from other lanthanides with the simplified technique of high performance liquid chromatography (HPLC) system. The separation time of Pm and Sm in HPLC separation was shortened by stepwise eluent method of α-hydroxyisobutyric acid as compared with a gradient eluent method of lactic acid with HPLC despite increase in sample volume for significant determination of Pm-147 and Sm-151. This method permitted the detection limit around 0.1 Bq/kg-dry-soil for Pm-147 and Sm-151 in 200 g soil sample by counting for 500 min with a liquid scintillation counter.