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Measurement uncertainty assessment for potentiometric determination of trace anionic impurities in graphite post ultrasonic extraction: A bottom-up approach 超声提取后石墨中微量阴离子杂质电位测定的测量不确定度评定:自下而上方法
IF 1.3 Q3 Chemistry Pub Date : 2022-05-07 DOI: 10.25135/jcm.69.2202.2367
H. Parab, Sangita D. Kumar
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引用次数: 0
Identification, separation and mass spectral characterization of degradants in Cariprazine HCl by LC-MS/MS/QTOF LC-MS/MS/QTOF法鉴定、分离盐酸卡里吡嗪中降解物及质谱表征
IF 1.3 Q3 Chemistry Pub Date : 2022-05-01 DOI: 10.25135/jcm.68.2201.2338
Pallekona Sushma, A. Pawar
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引用次数: 2
LC-HRMS profiling of phytochemicals, antidiabetic, anticholinergic and antioxidant activities of evaporated ethanol extract of Astragalus brachycalyx Fischer LC-HRMS分析短枝黄芪蒸发乙醇提取物的植物化学物质、抗糖尿病、抗胆碱能和抗氧化活性
IF 1.3 Q3 Chemistry Pub Date : 2021-12-26 DOI: 10.25135/jcm.62.2107.2155
I. Gülçin, Hatice Kiziltaş, Zeynebe Bi̇ngöl, A. Gören, S. M. Pinar, S. Alwasel
Astragalus is a perennial plant that has existed for about 2500-3000 years and consists of more than 250 taxonomic parts. Twenty species of Astragalus are endemic to Turkey, as well as the richest genus with 425 taxa. The roots of Astragalus species are used in folk medicine as hepatoprotective, antioxidant, antibacterial, antihypertensive, antidiabetic and diuretic. Also, it is used to treat diabetes mellitus, leukemia, nephritis and uterine cancer. It is known that in Anatolia, Astragalus roots are traditionally used against leukemia and wound healing. For the purpose, the measuring of antioxidant activity of evaporated ethanol extract of Astragalus brachycalyx FISCHER (EEAB), some bioanalytic methods including DPPH and ABTS scavenging effects, ferric ions (Fe) and cupric ions (Cu) reducing abilities, and metal (Fe) chelating activity were realized. α-Tocopherol, ascorbic acid, and BHT were used as the standard antioxidants. On the other hand, some phenolic compounds, which responsible for antioxidant activities of EEAB was determined by liquid chromatography-high resolution mass spectrometry (LC-HRMS). At the similar concentration, EEAB exhibited efficient antioxidant effects when compared to standard compounds. Additionally, EEAB showed IC50 values of 1.985 μg/mL toward acetylcholinesterase (AChE), 0.620 μg/mL on α-glycosidase and 0.306 μg/mL against α-amylase enzymes.
黄芪是一种多年生植物,已有2500-3000年的历史,由250多个分类部分组成。20种黄芪是土耳其的特有种,也是最丰富的属,有425个分类群。黄芪的根在民间医学中具有保肝、抗氧化、抗菌、降压、抗糖尿病和利尿的作用。此外,它还用于治疗糖尿病,白血病,肾炎和子宫癌症。众所周知,在安纳托利亚,黄芪根传统上用于治疗白血病和伤口愈合。为此,实现了短枝黄芪蒸发乙醇提取物(EEAB)抗氧化活性的测定,包括DPPH和ABTS的清除作用、铁离子(Fe)和铜离子(Cu)的还原能力以及金属(Fe)螯合活性等生物分析方法。α-生育酚、抗坏血酸和BHT作为标准抗氧化剂。另一方面,采用液相色谱-高分辨质谱法(LC-HRMS)测定了EEAB抗氧化活性的一些酚类化合物。在相似的浓度下,与标准化合物相比,EEAB表现出有效的抗氧化作用。此外,EEAB对乙酰胆碱酯酶(AChE)的IC50值为1.985μg/mL,对α-糖苷酶的IC50为0.620μg/mL。
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引用次数: 15
Development of a quality control material for the analysis of volatile compounds in alcoholic beverages 用于分析酒精饮料中挥发性化合物的质量控制材料的开发
IF 1.3 Q3 Chemistry Pub Date : 2021-12-26 DOI: 10.25135/jcm.66.2111.2259
S. Charapitsa, S. Sytova, A. Kavalenka, L. Sobolenko, Yauheni Shauchenka, N. Kostyuk, M. Zayats, V. Egorov, S. Leschev, I. Melsitova, Siarhei Vetokhin, N. Zayats
: A quality control material (QCM) for the analysis of volatile compounds in alcoholic beverages was developed. The problems of the development and production of QCM were investigated. The seven water-ethanol solutions, containing 9 volatile compounds (acetaldehyde, methyl acetate, ethyl acetate, methanol, propan-1-ol, propan-2-ol, 2-methylpropan-1-ol, butan-1-ol and 3-methylbutan-1-ol) with a concentration range from 1.20 to 5000 mg/L of anhydrous ethanol were prepared and studied according to the ISO Guide 80 and ISO Guide 35 in order to prove their stability over 6 months. The algorithm for the assessment of uncertainty associated with the characterization of QCM was developed. The studies were carried out by validated direct gas chromatography (GC) method with flame ionization detection (FID), based on using ethanol as an internal standard. The expanded relative uncertainty of QCM does not exceed 4.5 %.
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引用次数: 3
SSimultaneous estimation of Pyridoxine HCl and FMOC-Leucine using derivative and chromatographic approach in pharmaceutical dosage form 药物剂型中盐酸吡哆醇和fmoc -亮氨酸的衍生色谱法同时测定
IF 1.3 Q3 Chemistry Pub Date : 2021-12-17 DOI: 10.25135/jcm.65.2109.2205
Dr Akhil Nagar, Chaitali R Patel, P. Jain, Samadhan J. Shinde, A. Shirkhedkar, Ruchita Bardya
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引用次数: 3
Characterization of low-density polyethylene reference material for melt flow rate by collaboration of NIS and a network of competent laboratories NIS和主管实验室网络合作对低密度聚乙烯熔体流动速率参考材料的表征
IF 1.3 Q3 Chemistry Pub Date : 2021-10-10 DOI: 10.25135/jcm.63.2107.2148
H. Moustafa, Ibrahim F. Tahoun, A. Abou‐Kandil, N. Darwish
The growth rate of plastic manufacturing all over the world and in the middle east as oil producing countries increased the rate of thermoplastics production and the needs of reference materials (RMs) for use in performance evaluation of measuring instruments and ensuring validity of measurement results. This article was focused on the preparation of RM based melt mass-flow rate from low-density polyethylene (LDPE) according to ISO 1133-1 standard. The characterization was evaluated from around 10% of prepared units, then the samples were distributed to a network of collaborating laboratories in order to ensure the validity of the RM production process. The value of melt mass-flow rate of LDPE was determined to be 19.51 g/10 min under a temperature of 190°C and a load of 2.16 kg with expanded uncertainty 0.38 at 95% confidence level. The obtained values were confirmed from the data reported by the network of collaborating laboratories.
世界各地和中东地区塑料制造业的增长率,因为石油生产国提高了热塑性塑料的生产率,并增加了用于测量仪器性能评估和确保测量结果有效性的参考材料(RM)的需求。本文根据ISO 1133-1标准,以低密度聚乙烯(LDPE)为原料,制备了基于RM的熔体质量流量。对约10%的制备单元进行了表征评估,然后将样品分发给合作实验室网络,以确保RM生产过程的有效性。在190°C的温度和2.16kg的载荷下,LDPE的熔体质量流速值被确定为19.51g/10min,在95%置信水平下的扩展不确定度为0.38。从合作实验室网络报告的数据中确认了获得的值。
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引用次数: 1
Quantification of antileukemic drug Dasatinib in human plasma: Application of a sensitive liquid chromatographic method 人血浆中抗白血病药物达沙替尼的定量:灵敏液相色谱法的应用
IF 1.3 Q3 Chemistry Pub Date : 2021-10-09 DOI: 10.25135/jcm.64.2108-2174
Avani Chokshi, A. Gajjar, Pooja Bhanushali, Pritesh Desai
Dasatinib is a tyrosine kinase inhibitor that is approved and prescribed to patients with chronic myelogenous leukemia and Philadelphia chromosome. Present work reports development of reversed-phase high performance liquid chromatographic method for determination of Dasatinib in human plasma and validation of the developed method according to the guidelines provided by European Medicines Agency (EMA). An RP-HPLC method with UV detection and isocratic elution has been developed and validated for analysis of Dasatinib in human plasma over a range of 5-300 ng/mL. Imatinib was used as an internal standard. Both, the drug and the internal standard were separated on the Inertsil C18 column (150 mm×4.6 mm×0.005 mm) using Ammonium Acetate buffer pH 6.4 and acetonitrile at a ratio of 65:35 as mobile phase. The flow rate was adjusted to 0.7 mL min-1. The detection was performed at 310 nm wavelength. Sample pre-purification was performed through simple protein precipitation using acetonitrile followed by sample collection through centrifugation. The developed method was linear in the range of 5-300 ng/mL with correlation coefficients (r) of 0.995. The lower limit of quantification for Dasatinib in plasma was 5 ng/mL. The accuracy and precision of the method were well within the acceptable limits of 15% over the linear range. In general, the developed method is efficient and inexpensive. It is very simple from the extraction of drug from the plasma matrix to the isocratic elution of analytes. From the data, it can be concluded that the developed method is selective, precise and accurate and applicable for the determination of Dasatinib in human plasma samples.
达沙替尼是一种酪氨酸激酶抑制剂,被批准用于慢性粒细胞白血病和费城染色体患者。目前的工作报告了用于测定人血浆中达沙替尼的反相高效液相色谱法的开发,并根据欧洲药品管理局(EMA)提供的指南对所开发的方法进行了验证。已经开发并验证了一种具有UV检测和等度洗脱的RP-HPLC方法,用于分析5-300 ng/mL范围内的人血浆中的达沙替尼。伊马替尼被用作内标。药物和内标物均在Inertsil C18柱(150mm×4.6mm×0.005mm)上分离,使用醋酸铵缓冲液pH 6.4和乙腈(比例为65:35)作为流动相。将流速调节至0.7 mL min-1。检测波长为310nm。样品预纯化通过使用乙腈的简单蛋白质沉淀进行,然后通过离心收集样品。所开发的方法在5-300 ng/mL范围内呈线性,相关系数(r)为0.995。达沙替尼在血浆中的定量下限为5 ng/mL。该方法的准确度和精密度在线性范围内均在15%的可接受范围内。总的来说,所开发的方法是有效和廉价的。从血浆基质中提取药物到分析物的等度洗脱非常简单。从数据中可以得出结论,该方法具有选择性、精确性和准确性,适用于人血浆样品中达沙替尼的测定。
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引用次数: 2
Development of a quick reverse phase liquid chromatographic method with photodiode-array detection for quantitative determination of chlorthalidone, metoprolol succinate and telmisartan in tablet formulation 光电二极管阵列快速反相液相色谱法测定片剂中氯噻酮、琥珀酸美托洛尔和替米沙坦的含量
IF 1.3 Q3 Chemistry Pub Date : 2021-08-24 DOI: 10.25135/jcm.6012106.2098
Avani Chokshi, R. Prajapati, Pritesh Desai, Mehul D. Patel
A quick and simple reversed-phase High-Performance Liquid Chromatographic method (RP-HPLC) with isocratic elution has been developed and validated for the concurrent quantitative determination of chlorthalidone, metoprolol succinate and telmisartan in the bulk mixture and tablet dosage form. The chromatographic separation was performed using Inertsil Octadecyl-Silica (ODSC18) Column (150mm×4.6mm, 5μm) stationary phase. The separation and elution was carried out using a mobile phase mixture of phosphate buffer (50 mM, pH 2.5) and acetonitrile at a ratio of 40:60 v/v and 0.7 mL/min flow rate. Chlorthalidone, metoprolol succinate and telmisartan were eluted at 2.96±0.5 min, 4.31±0.5 min and 5.94±0.5 min respectively. The response was recorded using a photodiode array (PDA) detector at 225 nm wavelength. The selected method was linear in the range of 3.21-18.72 μg/mL, 6.25-37.50 μg/mL and 10-60 μg/mL while percentage recovery was in the range from 99.15 to 99.93%, 99.15 to 99.42% and 100.03 to 100.08% for chlorthalidone, metoprolol succinate and telmisartan respectively. The method was found to be sensitive, selective, linear and reproducible and the results obtained suggest the suitability of the developed method for routine analysis of the formulations containing the combination of these drugs.
建立了一种快速简便的反相高效液相色谱法(RP-HPLC),用于同时定量测定原料药和片剂中氯噻酮、琥珀酸美托洛尔和替米沙坦的含量。采用Inertsil Octadecyl-Silica (ODSC18)柱(150mm×4.6mm, 5μm)固定相进行色谱分离。采用磷酸缓冲液(50 mM, pH 2.5)与乙腈的流动相混合物,以40:60 v/v和0.7 mL/min流速进行分离和洗脱。氯噻酮、琥珀酸美托洛尔和替米沙坦洗脱时间分别为2.96±0.5 min、4.31±0.5 min和5.94±0.5 min。利用光电二极管阵列(PDA)探测器在225 nm波长处记录响应。所选方法在3.21 ~ 18.72 μg/mL、6.25 ~ 37.50 μg/mL和10 ~ 60 μg/mL范围内呈线性关系,氯噻酮、琥珀酸美托洛尔和替米沙坦的回收率分别为99.15 ~ 99.93%、99.15 ~ 99.42%和100.03 ~ 100.08%。结果表明,该方法具有灵敏度高、选择性好、线性好、重复性好等特点,适用于复方制剂的常规分析。
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引用次数: 1
Isolation of amygdalin epimer at high diastereomeric purity and its structural characterization by spectroscopic and Q-TOF LC-MS methods 高非对映异构体纯度苦杏仁苷表聚体的分离及其光谱和Q-TOF LC-MS表征
IF 1.3 Q3 Chemistry Pub Date : 2021-08-18 DOI: 10.25135/jcm.60.2105.2076
Irfan Capan, S. Servi, A. Aysal, Pshtiwan Raheem Sabır
Amygdalin, a cyanogenic glycoside mostly found in the bitter almond kernel, plays an important role in conventional and modern medicine applications. The high diastereomeric purity amygdalin was isolated with chromatographic purification methods and recrystallization. Amygdalin and neoamygdalin were separated chromatographically using the porous graphitic carbon column. Identification and confirmation of each molecule was performed with the ESI Quadrupole Time of Flight system coupled with a reversed phase LC.
苦杏仁苷是一种主要存在于苦杏仁中的发蓝糖苷,在传统和现代医学中发挥着重要作用。采用色谱纯化和重结晶的方法分离得到高非对映体纯度的苦杏仁苷。采用多孔石墨碳柱色谱分离苦杏仁苷和新苦杏仁苷。每个分子的鉴定和确认是用ESI四极飞行时间系统与反相LC耦合进行的。
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引用次数: 1
Stability indicating liquid chromatographic method for the estimation of remogliflozin etabonate 稳定性指示的液相色谱法测定瑞格列净的含量
IF 1.3 Q3 Chemistry Pub Date : 2020-12-01 DOI: 10.25135/jcm.46.20.07.1734
D. Shah, Ishita I. Gondalia, V. Patel, Ashok Mahajan, U. Chhalotiya
: Accurate and precise reverse phase liquid chromatographic method has been developed for the estimation Remogliflozin etabonate in bulk and tablet dosage form. Reverse phase C18 column was used as stationary phase along with mixture of methanol:water (70:30%, v/v) as a mobile phase. Mobile phase flow rate was maintained at 1mL/min and analysis was performed at 229 nm. The method was linear in the concentration range of 1 – 25 μg/mL with correlation coefficient (r 2 ) 0.997. The proposed method was validated with respect to linearity, accuracy, precision and robustness as per ICH Q2 (R1) guideline. To find out the possible degradation pathway, forced degradation studies were performed. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time value. The drug was found to be highly susceptible to acid and base hydrolysis. The developed method can be used for analysis of stability samples and routing quality control evaluation of Remogliflozin etabonate in
建立了准确、精确的反相液相色谱法测定安他巴酸雷莫列净散装剂型和片剂剂型的含量。以反相C18柱为固定相,甲醇:水(70:30%,v/v)为流动相。流动相流速保持在1mL/min,在229 nm进行分析。该方法在1 ~ 25 μg/mL浓度范围内线性良好,相关系数(r 2) 0.997。根据ICH Q2 (R1)指南对该方法进行了线性、准确度、精密度和鲁棒性验证。为了找出可能的降解途径,进行了强制降解研究。降解产物峰与纯药峰分离较好,保留时间差异显著。这种药物被发现对酸碱水解非常敏感。该方法可用于盐酸雷莫列净的稳定性样品分析和路线质量控制评价
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引用次数: 16
期刊
Journal of Chemical Metrology
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