A simple, rapid, specific and precise liquid chromatography—tandem mass spectrophotometric (LC-MS/MS) method was developed and validated for the quantification of chiral separated R-bicalutamide from S-bicalutamide, ...A simple, rapid, specific and precise liquid chromatography—tandem mass spectrophotometric (LC-MS/MS) method was developed and validated for the quantification of chiral separated R-bicalutamide from S-bicalutamide, in human plasma. Topiramate (TPM) was used as internal standard, added to plasma sample prior to extraction using t-butyl methyl ether (TBME). Chromatographic separation was achieved on CHIRALPAK AD-RH column (150 mm×4.6 mm, 5 μm) with acteonitrile: 0.1% formic acid Buffer (50:50 v/v) as an isocratic mobile phase with a flow rate of 1.0 mL·min-1. Quantitation was performed by transition of 429.0 → 255.0 (m/z) for R-bicalutamide and 338.1 → 77.8 (m/z) for topiramate. The lower limit of quantitation was 20 ng·mL-1with a 100 μL plasma sample. The concentrations of eight working standards showed linearity between 20 to 3200 ng·mL-1(r2≥ 0.9990). Chromatographic separation was achieved within 6 min, compared to the 15 min of previous methods. The average extraction recoveries of 3 quality control concentrations were 98.56% for R-bicalutamide and 92.42% for topiramate. The coefficient of variation was ≤15% for intra- and inter-batch assays. Therefore a rapid, specific and sensitive LC-MS/MS method for the quantification of R-bicalutamide in human plasma was developed and validated can be used in the bioequivalence study of this drug.展开更多
Benzene derivatives are volatile organic compounds commonly present in the atmospheric environment,which are toxic and complex in composition.They have become a key regulatory object in China s atmospheric environment...Benzene derivatives are volatile organic compounds commonly present in the atmospheric environment,which are toxic and complex in composition.They have become a key regulatory object in China s atmospheric environment management.In this paper,Shimadzu Nexis GC-2030 gas chromatography was used to simultaneously detect eight benzene derivatives.According to the Environmental Monitoring—Technical Guideline on Drawing and Revising Analytical Method Standards(HJ 168-2010),the monitoring methods for benzene,toluene,ethylbenzene,p-xylene,m-xylene,isopropylbenzene,o-xylene,and styrene in the Stationary Source Emission—Determination of Benzene and Its Analogies—Bags Sampling/Direct Injection—Gas Chromatography(HJ 1261-2022)are verified,and their linear relationships,detection limits,precision and accuracy are analyzed.展开更多
[Objective] This study was conducted to establish a microbial limit test method for Bupi Qiangli Ointment. [Method] The conventional method and medium dilution method were used for bacterial, mold and yeast counting i...[Objective] This study was conducted to establish a microbial limit test method for Bupi Qiangli Ointment. [Method] The conventional method and medium dilution method were used for bacterial, mold and yeast counting in sample recovery test. [Result] The medium dilution method （1：10 test solution, 0.5 ml/plate） could effectively eliminate the inhibition effect of the Bupi Qiangli Ointment, and the recovery of Staphylococcus aureus was greater than 70% in the 3 batches of samples; and the conventional method exhibited the recoveries of E. coil, Bacillus subtilis, Candida albicans and Aspergillus greater than 70% in the 3 batches of samples. [Conclusion] Due to Bupi Qiangli Ointment has strongly antibacterial effect on Staphylococcus au- reus, the medium dilution method was used for bacterial counting, and the conventional method was used for mold and yeast counting; and the conventional method was used for controlled bacterium examination of E. coll.展开更多
In this paper, the many indices used in validation of crop models, such as RMSE （root mean square errors）, Sd （standard error of absolute difference）, da （mean absolute difference）, dap （ratio of da to the mean...In this paper, the many indices used in validation of crop models, such as RMSE （root mean square errors）, Sd （standard error of absolute difference）, da （mean absolute difference）, dap （ratio of da to the mean observation）, r （correlation）, and R2 （determination coefficient）, are compared for the same rice architectural parameter model, and their advantages and disadvantages are analyzed. A new index for validation of crop models, dap between the observed and the simulated values, is proposed, with dap〈5% as the suggested standard for precision of crop models. The different kinds of validation methods in crop models should be combined in the following aspects：（1） calculating da and dap; （2） calculating the RMSE or Sd; （3） calculating r and R2, at the same time, plotting 1：1 diagram.展开更多
Geological disasters not only cause economic losses and ecological destruction, but also seriously threaten human survival. Selecting an appropriate method to evaluate susceptibility to geological disasters is an impo...Geological disasters not only cause economic losses and ecological destruction, but also seriously threaten human survival. Selecting an appropriate method to evaluate susceptibility to geological disasters is an important part of geological disaster research. The aims of this study are to explore the accuracy and reliability of multi-regression methods for geological disaster susceptibility evaluation, including Logistic Regression(LR), Spatial Autoregression(SAR), Geographical Weighted Regression(GWR), and Support Vector Regression(SVR), all of which have been widely discussed in the literature. In this study, we selected Yunnan Province of China as the research site and collected data on typical geological disaster events and the associated hazards that occurred within the study area to construct a corresponding index system for geological disaster assessment. Four methods were used to model and evaluate geological disaster susceptibility. The predictive capabilities of the methods were verified using the receiver operating characteristic(ROC) curve and the success rate curve. Lastly, spatial accuracy validation was introduced to improve the results of the evaluation, which was demonstrated by the spatial receiver operating characteristic(SROC) curve and the spatial success rate(SSR) curve. The results suggest that: 1) these methods are all valid with respect to the SROC and SSR curves, and the spatial accuracy validation method improved their modelling results and accuracy, such that the area under the curve(AUC) values of the ROC curves increased by about 3%–13% and the AUC of the success rate curve values increased by 15%–20%; 2) the evaluation accuracies of LR, SAR, GWR, and SVR were 0.8325, 0.8393, 0.8370 and 0.8539, which proved the four statistical regression methods all have good evaluation capability for geological disaster susceptibility evaluation and the evaluation results of SVR are more reasonable than others; 3) according to the evaluation results of SVR, the central-southern Yunnan Province are the highest sus-ceptibility areas and the lowest susceptibility is mainly located in the central and northern parts of the study area.展开更多
Distribution-based degradation models （or graphical approach in some literature） occur in a wide range of applications. However, few of existing methods have taken the validation of the built model into consideratio...Distribution-based degradation models （or graphical approach in some literature） occur in a wide range of applications. However, few of existing methods have taken the validation of the built model into consideration. A validation methodology for distribution-based models is proposed in this paper. Since the model can be expressed as consisting of assumptions of model structures and embedded model parameters, the proposed methodology carries out the validation from these two aspects. By using appropriate statistical techniques, the rationality of degradation distributions, suitability of fitted models and validity of degradation models are validated respectively. A new statistical technique based on control limits is also proposed, which can be implemented in the validation of degradation models＇ validity. The case study on degradation modeling of an actual accelerometer shows that the proposed methodology is an effective solution to the validation problem of distribution-based de qradation models.展开更多
<strong>Context:</strong> Substandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evalua...<strong>Context:</strong> Substandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evaluate the quality of tramadol in Kisangani before and during the Covid-19 period. <strong>Methods:</strong> For the analytical quantitative method, an experimental design was applied to set up the optimal levels of the selected factors, namely, pH of dissolution medium, type of cuvette, and wavelength. Taking into account the capsule pharmaceutical formulation within 80 - 120 μg·mL<sup>-1</sup> concentration range, we analyzed 89 tramadol samples from pharmacies and hospitals of the six Kisangani municipalities. <strong>Results:</strong> pH showed a significant effect on absorbance, whereas quartz cuvette and wavelength did not. A typical 100 μg·mL<sup>-1</sup> tramadol solution gave an absorbance of 0.64 at 272 nm. Validation highlighted a matrix effect observed with a 6% bias. A correction factor of 0.9372 allowed to improve the accuracy profile, which were then totally included within the 10% acceptance limits. Quality control revealed that 25 samples out of 89 were not compliant in terms of manufacturing license, registration status in DRC and content as well. <strong>Conclusion:</strong> This study showed that the strengthening of analytical strategy in Kisangani is a need.展开更多
The development of the extemporaneous preparations allows physicians to adjust the dose for pediatric patients and provides for a more convenient dosage vehicle for those patients with difficulty swallowing tablets[1]...The development of the extemporaneous preparations allows physicians to adjust the dose for pediatric patients and provides for a more convenient dosage vehicle for those patients with difficulty swallowing tablets[1].As such,the production unit of pharmacy division,Sappasit Prasong Hospital,Ubon Ratchathani province,prepared the extemporaneous formulations such as Acetazolamide(AM),Furosemide(FM)and Phenytoin(PT)powder for suspensions.The extemporaneous suspensions of 10 mg/mL AM,2 mg/mL FM and 10 mg/mL PT were prepared from 250 mg Diamox?,40 mg Lasix?and 50 mg Dilantin?tablets,respectively and diluted with syrup vehicle.展开更多
A modified ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitation of ibuprofen enantiomers in human plasma. Ibuprofen and flurbiprofen (in...A modified ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitation of ibuprofen enantiomers in human plasma. Ibuprofen and flurbiprofen (internal standard) were extracted from human plasma at acidic pH, using a single-step liquid-liquid extraction with methyl-tert-butyl ether. The enantiomers of ibuprofen and flurbiprofen were derivatized to yield the corresponding diastereomers. Chromatographic separation was achieved using a phenyl column with a run time of 20 min. (R)- and (S)-ibuprofen were quantitated at the multiple reaction monitoring (MRM) transition of m/z 360.2 ? 232.1, and (R)- and (S)-flurbiprofen were monitored at the MRM transition of m/z 398.3 ? 270.1. The method was validated for accuracy, precision, linearity, range, limit of quantitation (LOQ), limit of detection (LOD), selectivity, absolute recovery, matrix effect, dilution integrity, and evaluation of carry-over. Accuracy for (R)-ibuprofen ranged between –11.8% and 11.2%, and for (S)-ibuprofen between –8.6% and –0.3%. Precision for (R)-ibuprofen was ≤ 11.2%, and for (S)-ibuprofen ≤ 7.0%. The calibration curves were weighted (1/X2, n = 7) and were linear with r2 for (R)-ibuprofen ≥ 0.988 and for (S)-ibuprofen ≥ 0.990. The range of the method was 50 to 5000 ng/mL with the LOQ of 50 ng/mL, and LOD of 1 ng/mL, for (R)- and (S)-ibuprofen requiring 100 μL of sample. The method was applied successfully to a pharmacokinetic study with the administration of a single oral dose of ibuprofen capsules to human subjects.展开更多
In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one ...In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one antimalarial (quinine) and two antibiotics (amoxicillin and metronidazole) have been developed and validated according to the total error strategy using the accuracy profiles as a decision tool. The dosing range was 2 - 10 μg/mL (for quinine sulfate in tablet), 4 - 12 μg/mL (for quinine bichlorhydrate in oral drop-metronidazole benzaote in oral suspension) and 15 - 35 μg/mL (for amoxicillin trihydrate in capsule). The validated methods were then applied in determining the content of some analogous medicines sold in the Democratic Republic of Congo. Thus, the proposed UV-Visible spectrophotometric methods are simple and suitable to quantify quinine, amoxicillin and metronidazole in different pharmaceutical forms.展开更多
The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode arr...The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode array detector. The separation was done by using symmetry C-18 ODS (25 cm × 0.46 cm internal diameter) 5 μm analytical column containing mobile phase of Phosphate buffer (0.02 M) and methanol [65:35% v/v] adjusted pH to 4.8 by adding dilute ortho phosphoric acid. The method was run at 1 ml·min<sup>-1</sup> at 286 nm detection. The drug was eluted at 5.484 min. After developing the method, it was assured for the intended use by validation which was done according to ICH Q2B guidelines. The analytical parameters checked were linearity, accuracy, repeatability, intermediate precision, limit of detection, limit of quantitation, ruggedness and robustness. It was observed that the response of the detector was linear in the range of 6 - 14 μg/ml with correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability indicating assay method was established by using the samples generated by forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative and photolytic degradation and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the analysis of quality of the rucaparib drug.展开更多
The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar...The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The <i>λ</i><sub>max</sub> of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.展开更多
Cross iteration often exists in the computational process of the simulation models, especially for control models. There is a credibility defect tracing problem in the validation of models with cross iteration. In ord...Cross iteration often exists in the computational process of the simulation models, especially for control models. There is a credibility defect tracing problem in the validation of models with cross iteration. In order to resolve this problem, after the problem formulation, a validation theorem on the cross iteration is proposed, and the proof of the theorem is given under the cross iteration circumstance. Meanwhile, applying the proposed theorem, the credibility calculation algorithm is provided, and the solvent of the defect tracing is explained. Further, based on the validation theorem on the cross iteration, a validation method for simulation models with the cross iteration is proposed, which is illustrated by a flowchart step by step. Finally, a validation example of a sixdegree of freedom (DOF) flight vehicle model is provided, and the validation process is performed by using the validation method. The result analysis shows that the method is effective to obtain the credibility of the model and accomplish the defect tracing of the validation.展开更多
To analyze the spring disturbance torque caused by motionai cable harness in a stabilized platform, the Kirchhoff theory based cable harness model has been previously developed to dynamically simulate the motional cab...To analyze the spring disturbance torque caused by motionai cable harness in a stabilized platform, the Kirchhoff theory based cable harness model has been previously developed to dynamically simulate the motional cable harness. In this paper, this model was validated by comparing the simulation results with the experiment results （ both the spring force and the deformed profile of the motional cable harness）. In the experiment, a special optical measuring instrument based on binocular vision was developed and the motion and deformation of cable harness were measured. A simpli- fied stabilized platform system was constructed, and the absolute value of spring disturbance force during the motion of this simplified frame was obtained by using a force gauge （0. 02 N precision）. The physical parameters of experimental specimen were also measured. The experimental and simulated results showed good agreement. These results should be useful for better motional cable harness layout design and reliable evaluation of the spring disturbance torque.展开更多
The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cor...The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cortex (PFC) and blood sample of the rodents. In addition, using the hippocampus and standards of these three compounds we validated an isocratic fluorescence HPLC procedure for a simultaneous detection of them in a single chromatogram within a total run time of about 12 min. Reproducibility for TDP, TMP and B1 was 2.66%, 4.50% and 7.43% (intraday) and 37.54%, 25.39% and 25.87% (interday), respectively. Recovery assays were between 96.0% and 101.7%. The calibration curves were linear and the concentrations of the three compounds, all in nanomolar range, were determined in the brain areas and in the blood samples. When compared to the current methods in the literature, this new method provides information on essential variables, such as linearity range and limit of detection, reproducibility and stability of thiamine, TMP and TDP in rat brain samples. The present data on sample processing and B1 and its phosphate ester level determinations are the first to be validated using hippocampus samples of rats.展开更多
Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications ...Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications such as solriamfetol,which is used to treat excessive daytime sleepiness.Although the highperformance liquid chromatography analysis of commercial solriamfetol has revealed the presence of several impurities,their synthesis,structure elucidation,and chromatographic determination have not been reported yet.To bridge this gap,we herein identified,synthesized,and isolated eight processrelated solriamfetol impurities,characterized them using spectroscopic and chromatographic techniques,and proposed plausible mechanisms of their formation.Moreover,we developed and validated a prompt impurity analysis method based on ultrahigh-performance liquid chromatography with UV detection,revealing that its selectivity,linearity,accuracy,precision,and quantitation limit meet the acceptance criteria of method validation stipulated by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.Thus,the developed method was concluded to be suitable for the routine analysis of solriamfetol substances.展开更多
Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical ...Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical method variation parameters are based on pH variability of buffer solution of mobile phase, organic ratio composition changes, stationary phase (column) manufacture, brand name and lot number variation;flow rate variation and temperature variation of chromatographic system. The analytical chemical method for assay of Atropine Sulfate conducted for robustness evaluation. The typical variation considered for mobile phase organic ratio change, change of pH, change of temperature, change of flow rate, change of column etc. Purpose: The aim of this study is to develop a cost effective, short run time and robust analytical chemical method for the assay quantification of Atropine in Pharmaceutical Ophthalmic Solution. This will help to make analytical decisions quickly for research and development scientists as well as will help with quality control product release for patient consumption. This analytical method will help to meet the market demand through quick quality control test of Atropine Ophthalmic Solution and it is very easy for maintaining (GDP) good documentation practices within the shortest period of time. Method: HPLC method has been selected for developing superior method to Compendial method. Both the compendial HPLC method and developed HPLC method was run into the same HPLC system to prove the superiority of developed method. Sensitivity, precision, reproducibility, accuracy parameters were considered for superiority of method. Mobile phase ratio change, pH of buffer solution, change of stationary phase temperature, change of flow rate and change of column were taken into consideration for robustness study of the developed method. Results: The limit of quantitation (LOQ) of developed method was much low than the compendial method. The % RSD for the six sample assay of developed method was 0.4% where the % RSD of the compendial method was 1.2%. The reproducibility between two analysts was 100.4% for developed method on the contrary the compendial method was 98.4%.展开更多
Cinacalcet Hydrochloride (CIN) is a new calcimimetic agent indicated for the use in hypercalcemia. The present work is aimed at development and validation of a novel and simple high-performance thin-layer chromatograp...Cinacalcet Hydrochloride (CIN) is a new calcimimetic agent indicated for the use in hypercalcemia. The present work is aimed at development and validation of a novel and simple high-performance thin-layer chromatographic (HPTLC) method for the analysis of Cinacalcet Hydrochloride (active pharmaceutical ingredient, API. In the method, Aluminum-backed silica gel 60 F254 plates (10 × 10 cm) were used as stationary phase and chloroform: acetonitrile (6:4, v/v) as the mobile phase, which showed compact bands of Cinacalcet HCl (RF 0.30 ± 0.02). Quantitative analysis was carried out by densitometry at a wavelength of 282 nm. Linear regression analysis for the calibration spots showed good correlation ship with regression co-efficient r2 = 0.9994 in the range of 40 - 160 ng/band. The developed method suitability for quantification of CIN was learned by validating it as per the ICH guidelines. CIN detection limit was 0.48 ng/band and the quantification limit was 1.59 ng/band. The proposed method was found to be linear (r2 = 0.999), precise (%RSD < 2% for intraday and intermediate precision), accurate, specific, and robust. Further, the developed method was validated and found suitable for stress induced studies, since presence of degradants has no effect on CIN estimation. The proposed method was found to be simple, sensitive, precise, accurate and reproducible for the estimation of CIN.展开更多
A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. ...A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.展开更多
文摘A simple, rapid, specific and precise liquid chromatography—tandem mass spectrophotometric (LC-MS/MS) method was developed and validated for the quantification of chiral separated R-bicalutamide from S-bicalutamide, in human plasma. Topiramate (TPM) was used as internal standard, added to plasma sample prior to extraction using t-butyl methyl ether (TBME). Chromatographic separation was achieved on CHIRALPAK AD-RH column (150 mm×4.6 mm, 5 μm) with acteonitrile: 0.1% formic acid Buffer (50:50 v/v) as an isocratic mobile phase with a flow rate of 1.0 mL·min-1. Quantitation was performed by transition of 429.0 → 255.0 (m/z) for R-bicalutamide and 338.1 → 77.8 (m/z) for topiramate. The lower limit of quantitation was 20 ng·mL-1with a 100 μL plasma sample. The concentrations of eight working standards showed linearity between 20 to 3200 ng·mL-1(r2≥ 0.9990). Chromatographic separation was achieved within 6 min, compared to the 15 min of previous methods. The average extraction recoveries of 3 quality control concentrations were 98.56% for R-bicalutamide and 92.42% for topiramate. The coefficient of variation was ≤15% for intra- and inter-batch assays. Therefore a rapid, specific and sensitive LC-MS/MS method for the quantification of R-bicalutamide in human plasma was developed and validated can be used in the bioequivalence study of this drug.
文摘Benzene derivatives are volatile organic compounds commonly present in the atmospheric environment,which are toxic and complex in composition.They have become a key regulatory object in China s atmospheric environment management.In this paper,Shimadzu Nexis GC-2030 gas chromatography was used to simultaneously detect eight benzene derivatives.According to the Environmental Monitoring—Technical Guideline on Drawing and Revising Analytical Method Standards(HJ 168-2010),the monitoring methods for benzene,toluene,ethylbenzene,p-xylene,m-xylene,isopropylbenzene,o-xylene,and styrene in the Stationary Source Emission—Determination of Benzene and Its Analogies—Bags Sampling/Direct Injection—Gas Chromatography(HJ 1261-2022)are verified,and their linear relationships,detection limits,precision and accuracy are analyzed.
基金Supported by Traditional Chinese Medicine and Ethnic Minority Medicine Technology Research Subject of Guizhou Administrative Bureau(QZYY2013-70,QZYY-2014-026)Joint Application of Basic Research Fund of Science and Technology Department o Yunnan Province-Guiyang University of Chinese Medicine(QKHLHZ[2014]7323)~~
文摘[Objective] This study was conducted to establish a microbial limit test method for Bupi Qiangli Ointment. [Method] The conventional method and medium dilution method were used for bacterial, mold and yeast counting in sample recovery test. [Result] The medium dilution method （1：10 test solution, 0.5 ml/plate） could effectively eliminate the inhibition effect of the Bupi Qiangli Ointment, and the recovery of Staphylococcus aureus was greater than 70% in the 3 batches of samples; and the conventional method exhibited the recoveries of E. coil, Bacillus subtilis, Candida albicans and Aspergillus greater than 70% in the 3 batches of samples. [Conclusion] Due to Bupi Qiangli Ointment has strongly antibacterial effect on Staphylococcus au- reus, the medium dilution method was used for bacterial counting, and the conventional method was used for mold and yeast counting; and the conventional method was used for controlled bacterium examination of E. coll.
基金supported by the National High-Tech R&D Program (2006AA10Z230,2006AA10Z219-1)the National Natural Science Foundation of China (31171455)+3 种基金the Jiangsu Province Agricultural Scientific Technology Innovation Fund, China (CX(10)221, CX (11)2042)the Agricultural Scientific Technology Support Program, Jiangsu Province, China (BE2008397,BE2011342)the No-Profit Industry (Meteorology) Research Program, China (GYHY201006027, GYHY201106027)the Jiangsu Government Scholarship for Overseas Studies, China
文摘In this paper, the many indices used in validation of crop models, such as RMSE （root mean square errors）, Sd （standard error of absolute difference）, da （mean absolute difference）, dap （ratio of da to the mean observation）, r （correlation）, and R2 （determination coefficient）, are compared for the same rice architectural parameter model, and their advantages and disadvantages are analyzed. A new index for validation of crop models, dap between the observed and the simulated values, is proposed, with dap〈5% as the suggested standard for precision of crop models. The different kinds of validation methods in crop models should be combined in the following aspects：（1） calculating da and dap; （2） calculating the RMSE or Sd; （3） calculating r and R2, at the same time, plotting 1：1 diagram.
基金National Natural Science Foundation of China,No.41571077,No.41171318The Fundamental Research Funds for the Central Universities
文摘Geological disasters not only cause economic losses and ecological destruction, but also seriously threaten human survival. Selecting an appropriate method to evaluate susceptibility to geological disasters is an important part of geological disaster research. The aims of this study are to explore the accuracy and reliability of multi-regression methods for geological disaster susceptibility evaluation, including Logistic Regression(LR), Spatial Autoregression(SAR), Geographical Weighted Regression(GWR), and Support Vector Regression(SVR), all of which have been widely discussed in the literature. In this study, we selected Yunnan Province of China as the research site and collected data on typical geological disaster events and the associated hazards that occurred within the study area to construct a corresponding index system for geological disaster assessment. Four methods were used to model and evaluate geological disaster susceptibility. The predictive capabilities of the methods were verified using the receiver operating characteristic(ROC) curve and the success rate curve. Lastly, spatial accuracy validation was introduced to improve the results of the evaluation, which was demonstrated by the spatial receiver operating characteristic(SROC) curve and the spatial success rate(SSR) curve. The results suggest that: 1) these methods are all valid with respect to the SROC and SSR curves, and the spatial accuracy validation method improved their modelling results and accuracy, such that the area under the curve(AUC) values of the ROC curves increased by about 3%–13% and the AUC of the success rate curve values increased by 15%–20%; 2) the evaluation accuracies of LR, SAR, GWR, and SVR were 0.8325, 0.8393, 0.8370 and 0.8539, which proved the four statistical regression methods all have good evaluation capability for geological disaster susceptibility evaluation and the evaluation results of SVR are more reasonable than others; 3) according to the evaluation results of SVR, the central-southern Yunnan Province are the highest sus-ceptibility areas and the lowest susceptibility is mainly located in the central and northern parts of the study area.
文摘Distribution-based degradation models （or graphical approach in some literature） occur in a wide range of applications. However, few of existing methods have taken the validation of the built model into consideration. A validation methodology for distribution-based models is proposed in this paper. Since the model can be expressed as consisting of assumptions of model structures and embedded model parameters, the proposed methodology carries out the validation from these two aspects. By using appropriate statistical techniques, the rationality of degradation distributions, suitability of fitted models and validity of degradation models are validated respectively. A new statistical technique based on control limits is also proposed, which can be implemented in the validation of degradation models＇ validity. The case study on degradation modeling of an actual accelerometer shows that the proposed methodology is an effective solution to the validation problem of distribution-based de qradation models.
文摘<strong>Context:</strong> Substandard and falsified medicines are circulating in low-income countries mostly without any control. We availed a simple and not expensive UV-Vis spectroscopic method to evaluate the quality of tramadol in Kisangani before and during the Covid-19 period. <strong>Methods:</strong> For the analytical quantitative method, an experimental design was applied to set up the optimal levels of the selected factors, namely, pH of dissolution medium, type of cuvette, and wavelength. Taking into account the capsule pharmaceutical formulation within 80 - 120 μg·mL<sup>-1</sup> concentration range, we analyzed 89 tramadol samples from pharmacies and hospitals of the six Kisangani municipalities. <strong>Results:</strong> pH showed a significant effect on absorbance, whereas quartz cuvette and wavelength did not. A typical 100 μg·mL<sup>-1</sup> tramadol solution gave an absorbance of 0.64 at 272 nm. Validation highlighted a matrix effect observed with a 6% bias. A correction factor of 0.9372 allowed to improve the accuracy profile, which were then totally included within the 10% acceptance limits. Quality control revealed that 25 samples out of 89 were not compliant in terms of manufacturing license, registration status in DRC and content as well. <strong>Conclusion:</strong> This study showed that the strengthening of analytical strategy in Kisangani is a need.
文摘The development of the extemporaneous preparations allows physicians to adjust the dose for pediatric patients and provides for a more convenient dosage vehicle for those patients with difficulty swallowing tablets[1].As such,the production unit of pharmacy division,Sappasit Prasong Hospital,Ubon Ratchathani province,prepared the extemporaneous formulations such as Acetazolamide(AM),Furosemide(FM)and Phenytoin(PT)powder for suspensions.The extemporaneous suspensions of 10 mg/mL AM,2 mg/mL FM and 10 mg/mL PT were prepared from 250 mg Diamox?,40 mg Lasix?and 50 mg Dilantin?tablets,respectively and diluted with syrup vehicle.
文摘A modified ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitation of ibuprofen enantiomers in human plasma. Ibuprofen and flurbiprofen (internal standard) were extracted from human plasma at acidic pH, using a single-step liquid-liquid extraction with methyl-tert-butyl ether. The enantiomers of ibuprofen and flurbiprofen were derivatized to yield the corresponding diastereomers. Chromatographic separation was achieved using a phenyl column with a run time of 20 min. (R)- and (S)-ibuprofen were quantitated at the multiple reaction monitoring (MRM) transition of m/z 360.2 ? 232.1, and (R)- and (S)-flurbiprofen were monitored at the MRM transition of m/z 398.3 ? 270.1. The method was validated for accuracy, precision, linearity, range, limit of quantitation (LOQ), limit of detection (LOD), selectivity, absolute recovery, matrix effect, dilution integrity, and evaluation of carry-over. Accuracy for (R)-ibuprofen ranged between –11.8% and 11.2%, and for (S)-ibuprofen between –8.6% and –0.3%. Precision for (R)-ibuprofen was ≤ 11.2%, and for (S)-ibuprofen ≤ 7.0%. The calibration curves were weighted (1/X2, n = 7) and were linear with r2 for (R)-ibuprofen ≥ 0.988 and for (S)-ibuprofen ≥ 0.990. The range of the method was 50 to 5000 ng/mL with the LOQ of 50 ng/mL, and LOD of 1 ng/mL, for (R)- and (S)-ibuprofen requiring 100 μL of sample. The method was applied successfully to a pharmacokinetic study with the administration of a single oral dose of ibuprofen capsules to human subjects.
文摘In the framework of fighting against the poor quality medicines sold in developing countries using classical analytical methods easily accessible in those countries, four UV-Visible spectrophotometric methods for one antimalarial (quinine) and two antibiotics (amoxicillin and metronidazole) have been developed and validated according to the total error strategy using the accuracy profiles as a decision tool. The dosing range was 2 - 10 μg/mL (for quinine sulfate in tablet), 4 - 12 μg/mL (for quinine bichlorhydrate in oral drop-metronidazole benzaote in oral suspension) and 15 - 35 μg/mL (for amoxicillin trihydrate in capsule). The validated methods were then applied in determining the content of some analogous medicines sold in the Democratic Republic of Congo. Thus, the proposed UV-Visible spectrophotometric methods are simple and suitable to quantify quinine, amoxicillin and metronidazole in different pharmaceutical forms.
文摘The research was carried out for establishing a new reverse phase-HPLC stability indicating method for the quantification of Rucaparib. The experiment was determined on Waters HPLC instrument using 996 photo-diode array detector. The separation was done by using symmetry C-18 ODS (25 cm × 0.46 cm internal diameter) 5 μm analytical column containing mobile phase of Phosphate buffer (0.02 M) and methanol [65:35% v/v] adjusted pH to 4.8 by adding dilute ortho phosphoric acid. The method was run at 1 ml·min<sup>-1</sup> at 286 nm detection. The drug was eluted at 5.484 min. After developing the method, it was assured for the intended use by validation which was done according to ICH Q2B guidelines. The analytical parameters checked were linearity, accuracy, repeatability, intermediate precision, limit of detection, limit of quantitation, ruggedness and robustness. It was observed that the response of the detector was linear in the range of 6 - 14 μg/ml with correlation coefficient of 0.999. The results of all the parameters were found to be within the acceptance criteria. The stability indicating assay method was established by using the samples generated by forced degradation process. The forced degradation was carried out by subjecting the drug to acid, alkali, thermal, oxidative and photolytic degradation and the results showed that the degradation products were successfully separated from the drug. Hence, this can be applied perfectly later for the analysis of quality of the rucaparib drug.
文摘The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The <i>λ</i><sub>max</sub> of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.
基金supported by the National Natural Science Foundation of China(61374164)
文摘Cross iteration often exists in the computational process of the simulation models, especially for control models. There is a credibility defect tracing problem in the validation of models with cross iteration. In order to resolve this problem, after the problem formulation, a validation theorem on the cross iteration is proposed, and the proof of the theorem is given under the cross iteration circumstance. Meanwhile, applying the proposed theorem, the credibility calculation algorithm is provided, and the solvent of the defect tracing is explained. Further, based on the validation theorem on the cross iteration, a validation method for simulation models with the cross iteration is proposed, which is illustrated by a flowchart step by step. Finally, a validation example of a sixdegree of freedom (DOF) flight vehicle model is provided, and the validation process is performed by using the validation method. The result analysis shows that the method is effective to obtain the credibility of the model and accomplish the defect tracing of the validation.
基金Supported by the National Natural Science Foundation of China(50805009)
文摘To analyze the spring disturbance torque caused by motionai cable harness in a stabilized platform, the Kirchhoff theory based cable harness model has been previously developed to dynamically simulate the motional cable harness. In this paper, this model was validated by comparing the simulation results with the experiment results （ both the spring force and the deformed profile of the motional cable harness）. In the experiment, a special optical measuring instrument based on binocular vision was developed and the motion and deformation of cable harness were measured. A simpli- fied stabilized platform system was constructed, and the absolute value of spring disturbance force during the motion of this simplified frame was obtained by using a force gauge （0. 02 N precision）. The physical parameters of experimental specimen were also measured. The experimental and simulated results showed good agreement. These results should be useful for better motional cable harness layout design and reliable evaluation of the spring disturbance torque.
文摘The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cortex (PFC) and blood sample of the rodents. In addition, using the hippocampus and standards of these three compounds we validated an isocratic fluorescence HPLC procedure for a simultaneous detection of them in a single chromatogram within a total run time of about 12 min. Reproducibility for TDP, TMP and B1 was 2.66%, 4.50% and 7.43% (intraday) and 37.54%, 25.39% and 25.87% (interday), respectively. Recovery assays were between 96.0% and 101.7%. The calibration curves were linear and the concentrations of the three compounds, all in nanomolar range, were determined in the brain areas and in the blood samples. When compared to the current methods in the literature, this new method provides information on essential variables, such as linearity range and limit of detection, reproducibility and stability of thiamine, TMP and TDP in rat brain samples. The present data on sample processing and B1 and its phosphate ester level determinations are the first to be validated using hippocampus samples of rats.
基金This research was funded by the Deanship of Scientific Research at the German-Jordanian University and the Deanship of Scientific Research at Zarqa University.The graphical abstract was created with BioRender software.
文摘Given that impurities may affect the quality and safety of drug products,impurity identification and profiling is an integral part of drug quality control and is particularly important for newly developed medications such as solriamfetol,which is used to treat excessive daytime sleepiness.Although the highperformance liquid chromatography analysis of commercial solriamfetol has revealed the presence of several impurities,their synthesis,structure elucidation,and chromatographic determination have not been reported yet.To bridge this gap,we herein identified,synthesized,and isolated eight processrelated solriamfetol impurities,characterized them using spectroscopic and chromatographic techniques,and proposed plausible mechanisms of their formation.Moreover,we developed and validated a prompt impurity analysis method based on ultrahigh-performance liquid chromatography with UV detection,revealing that its selectivity,linearity,accuracy,precision,and quantitation limit meet the acceptance criteria of method validation stipulated by the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.Thus,the developed method was concluded to be suitable for the routine analysis of solriamfetol substances.
文摘Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical method variation parameters are based on pH variability of buffer solution of mobile phase, organic ratio composition changes, stationary phase (column) manufacture, brand name and lot number variation;flow rate variation and temperature variation of chromatographic system. The analytical chemical method for assay of Atropine Sulfate conducted for robustness evaluation. The typical variation considered for mobile phase organic ratio change, change of pH, change of temperature, change of flow rate, change of column etc. Purpose: The aim of this study is to develop a cost effective, short run time and robust analytical chemical method for the assay quantification of Atropine in Pharmaceutical Ophthalmic Solution. This will help to make analytical decisions quickly for research and development scientists as well as will help with quality control product release for patient consumption. This analytical method will help to meet the market demand through quick quality control test of Atropine Ophthalmic Solution and it is very easy for maintaining (GDP) good documentation practices within the shortest period of time. Method: HPLC method has been selected for developing superior method to Compendial method. Both the compendial HPLC method and developed HPLC method was run into the same HPLC system to prove the superiority of developed method. Sensitivity, precision, reproducibility, accuracy parameters were considered for superiority of method. Mobile phase ratio change, pH of buffer solution, change of stationary phase temperature, change of flow rate and change of column were taken into consideration for robustness study of the developed method. Results: The limit of quantitation (LOQ) of developed method was much low than the compendial method. The % RSD for the six sample assay of developed method was 0.4% where the % RSD of the compendial method was 1.2%. The reproducibility between two analysts was 100.4% for developed method on the contrary the compendial method was 98.4%.
文摘Cinacalcet Hydrochloride (CIN) is a new calcimimetic agent indicated for the use in hypercalcemia. The present work is aimed at development and validation of a novel and simple high-performance thin-layer chromatographic (HPTLC) method for the analysis of Cinacalcet Hydrochloride (active pharmaceutical ingredient, API. In the method, Aluminum-backed silica gel 60 F254 plates (10 × 10 cm) were used as stationary phase and chloroform: acetonitrile (6:4, v/v) as the mobile phase, which showed compact bands of Cinacalcet HCl (RF 0.30 ± 0.02). Quantitative analysis was carried out by densitometry at a wavelength of 282 nm. Linear regression analysis for the calibration spots showed good correlation ship with regression co-efficient r2 = 0.9994 in the range of 40 - 160 ng/band. The developed method suitability for quantification of CIN was learned by validating it as per the ICH guidelines. CIN detection limit was 0.48 ng/band and the quantification limit was 1.59 ng/band. The proposed method was found to be linear (r2 = 0.999), precise (%RSD < 2% for intraday and intermediate precision), accurate, specific, and robust. Further, the developed method was validated and found suitable for stress induced studies, since presence of degradants has no effect on CIN estimation. The proposed method was found to be simple, sensitive, precise, accurate and reproducible for the estimation of CIN.
文摘A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.
