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药品分析方法验证要点的讨论 被引量:6
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作者 王思寰 吴越 +2 位作者 王玉 靳桂民 洪小栩 《药物分析杂志》 CAS CSCD 北大核心 2018年第9期1646-1651,共6页
分析方法验证是一个和分析方法建立相联系的过程,用于证明建立的方法及其参数满足分析应用要求。本文以《中华人民共和国药典》2015年版四部通则(9101)的验证内容为主线,对方法学验证中的一些要点进行了讨论。
关键词 分析方法验证 中华人民共和国药典 准确度 精密度 专属性 检测下限和定量下限 线性 范围 耐用性
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Estimation of cancer burden in Guangdong Province,China in 2009 被引量:3
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作者 Su-Mei Cao Yan-Jun Xu +4 位作者 Guo-Zhen Lin Qi-Hong Huang Kuang-Rong Wei Shang-Hang Xie Qing Liu 《Chinese Journal of Cancer》 SCIE CAS CSCD 2015年第12期594-601,共8页
Background:Surveying regional cancer incidence and mortality provides significant data that can assist in making health policy for local areas;however,the province- and region-based cancer burden in China is seldom re... Background:Surveying regional cancer incidence and mortality provides significant data that can assist in making health policy for local areas;however,the province- and region-based cancer burden in China is seldom reported.In this study,we estimated cancer incidence and mortality in Guangdong Province,China and presented basic information for making policies related to health resource allocation and disease control.Methods:A log-linear model was used to calculate the sex-,age-,and registry-specific ratios of incidence to mortality(l/M) based on cancer registry data from Guangzhou,Zhongshan,and Sihui between 2004 and 2008.The cancer incidences in 2009 were then estimated according to representative l/M ratios and the mortality records from eight death surveillance sites in Guangdong Province.The cancer incidences in each city were estimated by the corresponding sex- and age-specific incidences from cancer registries or death surveillance sites in each area.Finally,the total and region-based cancer incidences and mortalities for the entire population of Guangdong Province were summarized.Results:The estimated l/M ratios in Guangzhou(3.658),Zhongshan(2.153),and Sihui(1.527) were significantly different(P < 0.001),with an average l/M ratio of 2.446.Significant differences in the estimated l/M ratios were observed between distinct age groups and the three cancer registries.The estimated l/M ratio in females was significantly higher than that in males(2.864 vs.2.027,P < 0.001).It was estimated that there were 163,376 new cancer cases(99,689 males and 63,687 females) in 2009;it was further estimated that 115,049 people(75,054 males and 39,995females) died from cancer in Guangdong Province in 2009.The estimated crude and age-standardized rate of incidences(ASRI) in Guangdong Province were 231.34 and 246.87 per 100,000 males,respectively,and 156.98 and 163.57 per 100,000 females,respectively.The estimated crude and age-standardized rate of mortalities(ASRM) in Guangdong Province were 174.17 and 187.46 per 100,000 males,respectively,and 98.59 and 102.00 per 100,000 females,respectively.In comparison with the western area and the northern mountain area,higher ASRI and ASRM were recorded in the Pearl River Delta area and the eastern area in both males and females.Conclusions:Cancer imposes a heavy disease burden,and cancer patterns are unevenly distributed throughout Guangdong Province.More health resources should be allocated to cancer control,especially in the western and northern mountain areas. 展开更多
关键词 DISEASE burden Incidence-to-mortality ratio loq-linear model
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Development and Validation of a Method for Simultaneous Determination of Metformin Hydrochloride and Sitagliptin Phosphate in a Formulation by RP-HPLC 被引量:1
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作者 P. B. N. Prasad K. Satyanarayana G. Krishnamohan 《American Journal of Analytical Chemistry》 2014年第11期737-742,共6页
Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulat... Present study was aimed to develop and validate a reverse-phase high-performance liquid chromatography method for simultaneous determination of sitagliptin phosphate and metformin hy-drochloride in a marketed formulation. The drug separation was performed on Hibar-240, Li-chrosphere-100 C18 ODS (250 × 4.6 mm, 5 μm) column, at a flow rate of 1 mL/min. The mobile phase used was a mixture of methanol: potassium di-hydrogen phosphate buffer at a ratio of 70:30 v/v. The detection was carried out at a wavelength of 266 nm. The retention times of sitagliptin phosphate and metformin hydrochloride were found as 6.1 and 4.9 min respectively. Linear calibration curves with good correlation coefficients were obtained over the concentration ranges of 10 - 50 μg/mL for sitagliptin and 20 - 100 μg/mL for metformin. The limit of detection was 0.016 and 0.14 μg/mL and the limit of quantification was 0.048 and 0.42 μg/mL for sitagliptin phosphate and metformin hydrochloride respectively. Validation of the method demonstrated system selectivity, specificity, linearity, accuracy and precision. The developed method was found useful in the simultaneous analysis of sitagliptin phosphate and metformin hydrochloride in formulation. 展开更多
关键词 SITAGLIPTIN Phosphate METFORMIN HYDROCHLORIDE Reverse Phase High Performance Liquid Chromatography (RPHPLC) International Committee on HARMONIZATION (ICH) Guidelines LIMIT of Detection (LOD) LIMIT of QUANTITATION (LOQ) Linearity Precision Accuracy & Reproducibility
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Method Development and Validation for the Quantification of Acrylamide in Potato Chips and Other Locally Available Food by LC-MS/MS in Bangladesh
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作者 Mala Khan Md. Moniruzzaman Mamudul Hasan Razu 《Food and Nutrition Sciences》 2019年第7期876-892,共17页
A sensitive, precise, accurate and simple in house validated Liquid Chromatography and Tandem mass spectrometric (LC-MS/MS) analytical method was developed for the quantification of acrylamide in potato chips, a proba... A sensitive, precise, accurate and simple in house validated Liquid Chromatography and Tandem mass spectrometric (LC-MS/MS) analytical method was developed for the quantification of acrylamide in potato chips, a probable carcinogenic and neurotoxic compound in fried food items. Acrylamide was extracted and cleaned up by QuEChERS method, then analyzed by triple quadrupole mass spectrophotometer using positive electrospray-ionization mode and d3-Acrylamide internal standard. The analyte and internal standard were separated on a reversed-phase C18 column (100 × 2.0 mm, 2.5 μm) by gradient elution with water and methanol containing 0.1% formic acid as mobile phase. The analytical method was fully validated by assessment of linearity, specificity, precision, accuracy, selectivity and robustness with relative standard deviation of less than 4%. The calibration curves were found linear with correlation coefficient (r2) of 0.9997 over the concentration range 5 - 500 μg/L. The recoveries of Acrylamide in the concentration of 250, 400, and 500 μg/L were 97% to 104%. Based on the signal to noise ratio, the lower limit of detection (LOD) and lower limit of quantification (LOQ) were achieved 2.0 μg/L and 4.0 μg/L respectively. The proposed method was also applied to other available most popular 24 types of food (265 number of sample) first time in Bangladesh. The highest level of acrylamide has been found in fried products with the range of 197.04 μg/L to 114.63 μg/L, protein-rich food lies between 79.76 to 89.14 μg/L whereas baked food products exhibited less content in the range of 35.23 to 51.17 μg/L. 展开更多
关键词 LC-MS/MS ACRYLAMIDE LINEARITY Accuracy Precision LOD LOQ
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