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Method Validation and Measurement Uncertainty Estimation for Determination of Multiclass Pesticide Residues in Tomato by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) 利用液相色谱-串联质谱法(LC-MS/MS)测定番茄中多类农药残留的方法验证和测量不确定度估计
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-10 DOI: 10.1155/2024/3846392
Suraj Shrestha, Bandana Lamichhane, Nibedita Chaudhary
Method validation is an essential technique for ensuring the reliability and accuracy of an analytical method. This study aimed to optimize and validate a fast, reliable, and accurate method for quantitatively determining pesticide residues of diverse chemical classes in the tomato matrix. Various method performance characteristics were tested and compared with predefined criteria. Twenty-six different pesticides of diverse chemical classes were selected based on their use in tomato cultivation and the availability of reference materials. The pesticide residues in tomato samples were extracted with the QuEChERS technique with some modifications, followed by injection into an LC-MS/MS system operating in an optimized method. The validated method demonstrated reasonable specificity, as there were no interferences from matrix components at the retention times of pesticides. The calibration curves for all pesticides exhibited excellent linearities, with correlation coefficients exceeding 0.99. No significant matrix effect was observed for all pesticides in tomatoes, as the values fell within the range of ±20%. All pesticides were quantified successfully at a concentration of 5 μg/kg except for carbaryl, with an average recovery of more than 70% and a relative standard deviation of less than 20%. Similarly, measurement uncertainties were also estimated based on the validation data, and the values were found below the default limit of 50%. Subsequently, the validated method was applied to analyze 52 locally collected tomato samples. Study findings revealed that only four of the studied pesticides were detected in these samples, and their concentrations were below the maximum residue limits (500 µg/kg each for carbendazim, imidacloprid, and metalaxyl) established for tomatoes by the Government of Nepal and the Codex Alimentarius Commission.
方法验证是确保分析方法可靠性和准确性的重要技术。本研究旨在优化和验证一种快速、可靠、准确的方法,用于定量测定番茄基质中不同化学类别的农药残留。对各种方法的性能特征进行了测试,并与预定标准进行了比较。根据番茄种植中农药的使用情况和参考材料的可用性,选择了 26 种不同化学类别的农药。番茄样品中的农药残留采用 QuEChERS 技术提取,并进行了一些修改,然后注入 LC-MS/MS 系统,按照优化的方法进行操作。经过验证的方法具有合理的特异性,因为在农药的保留时间内没有基质成分的干扰。所有农药的校准曲线均表现出良好的线性,相关系数超过 0.99。番茄中的所有农药均未出现明显的基质效应,其数值均在±20%的范围内。除西维因外,所有农药在 5 μg/kg 浓度下都能成功定量,平均回收率超过 70%,相对标准偏差小于 20%。同样,还根据验证数据对测量不确定度进行了估计,发现其值低于 50%的默认限值。随后,该验证方法被用于分析 52 个本地采集的番茄样本。研究结果表明,在这些样品中只检测到四种所研究的农药,其浓度低于尼泊尔政府和食品法典委员会为番茄规定的最大残留限量(多菌灵、吡虫啉和甲霜灵各为 500 微克/千克)。
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引用次数: 0
Study on the Characteristics of Traditional Chinese Medicine Syndromes in Patients with Erosive Gastritis Based on Metabolomics 基于代谢组学的侵蚀性胃炎患者中医证候特征研究
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2024-01-02 DOI: 10.1155/2024/6684677
Zhang Shixiong, Liu Shaowei, Yang Zeqi, Xu Miaochan, Zhou Pingping, Bai Haiyan, Lv Jingjing, Wang Yangang
According to traditional Chinese medicine theory, tongue coatings reflect changes in the body. The goal of this study was to identify a metabolite or a set of metabolites capable of classifying characteristics of traditional Chinese medicine syndromes in erosive gastritis. In this study, we collected tongue coatings of patients with erosive gastritis with damp-heat syndrome (DHS), liver depression and qi stagnation syndrome (LDQSS), and healthy volunteers. Then, we analyzed the differences in metabolic characteristics between the two groups based on metabolomics. We identified 14 potential biomarkers related to the DHS group, and six metabolic pathways were enriched. The differential pathways included pyrimidine metabolism, pantothenate and CoA biosynthesis, citrate cycle (TCA cycle), pyruvate metabolism, glycolysis/gluconeogenesis, and purine metabolism. Similarly, in the LDQSS group, we identified 25 potential biomarkers and 18 metabolic pathways were enriched. The top five pathways were the TCA cycle, sphingolipid metabolism, fatty acid biosynthesis, pantothenate and CoA biosynthesis, and the pentose phosphate pathway. In conclusion, the DHS group and the LDQSS group have different characteristics.
根据传统中医理论,舌苔反映了身体的变化。本研究的目的是找出一种或一组能够对糜烂性胃炎的中医证候特征进行分类的代谢物。在这项研究中,我们采集了湿热蕴结证(DHS)、肝郁气滞证(LDQSS)糜烂性胃炎患者和健康志愿者的舌苔。然后,我们根据代谢组学分析了两组患者代谢特征的差异。我们发现了 14 个与 DHS 组相关的潜在生物标记物,并富集了 6 条代谢通路。这些差异途径包括嘧啶代谢、泛酸和 CoA 生物合成、柠檬酸循环(TCA 循环)、丙酮酸代谢、糖酵解/葡萄糖生成和嘌呤代谢。同样,在 LDQSS 组中,我们确定了 25 个潜在的生物标记物,并丰富了 18 个代谢途径。排在前五位的途径分别是 TCA 循环、鞘脂代谢、脂肪酸生物合成、泛酸和 CoA 生物合成以及磷酸戊糖途径。总之,DHS 组和 LDQSS 组具有不同的特征。
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引用次数: 0
Quantitative Analysis of Favipiravir by HPLC: Development and Validation 高效液相色谱法定量分析法维拉韦:开发与验证
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-31 DOI: 10.1155/2023/8847958
Moammal Qurt, Rania Eshtayyeh, Hani Naseef, Abdullah Rabba, Abdallah Damin Abukhalil, Numan Malkieh, Maher Kharouf
Favipiravir is a broad-spectrum oral antiviral agent and has been approved for the treatment of COVID-19 infection cases. It inhibits a protein known as RNA polymerase, which transcribes and replicates the viral RNA genome, causing the spread of the infection. The current study aimed to develop and validate a new analytical method utilizing HPLC in accordance with international requirements (ICH and FDA). The chromatographic conditions used to achieve good resolution and reproducibility were a mixture of acetonitrile and 0.1% phosphoric acid buffer in the ratio of 60 : 40 v/v as the mobile phase. The flow rate was 1.0 mL/min, the wavelength (λ) was determined at 250 nm, and a retention time was approximately 3 minutes for favipiravir. The HPLC analysis was performed on the Dionex 300 system equipped with a Phenomenex C8 (250 cm 4.6 mm) 5 μm column. The total runtime was 6.0 min. The findings indicated that the method had been validated satisfactorily. Across the concentration range of 0.10–0.75 mg/ml, the calibration curve revealed a linear relationship. The accuracy of the current method was to be 99.2%. The limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.013 ppm, respectively. The standard and sample solution repeatability tests revealed that the procedure was precise and within acceptable ranges. The RSD% for the determination of precision was <2%. The results for robustness and solution stability were within acceptable limits. Finally, the new method provided an excellent result for all analytical method validation parameters and met the acceptance criteria. In addition, the new approach has a short run time and a retention time of around 4 minutes.
法维拉韦是一种广谱口服抗病毒药物,已被批准用于治疗 COVID-19 感染病例。它能抑制一种被称为 RNA 聚合酶的蛋白质,RNA 聚合酶负责转录和复制病毒 RNA 基因组,从而导致感染扩散。本研究旨在根据国际要求(ICH 和 FDA),利用高效液相色谱法开发并验证一种新的分析方法。为获得良好的分辨率和重现性,采用的色谱条件是乙腈和 0.1% 磷酸缓冲液的混合物,比例为 60 :40 v/v 的混合液作为流动相。流速为 1.0 mL/min,波长 (λ) 为 250 nm,法非拉韦的保留时间约为 3 分钟。高效液相色谱分析在配备了 Phenomenex C8 (250 cm 4.6 mm) 5 μm 色谱柱的 Dionex 300 系统上进行。总运行时间为 6.0 分钟。结果表明,该方法的验证结果令人满意。在 0.10-0.75 mg/ml 的浓度范围内,校准曲线呈线性关系。该方法的准确度为 99.2%。检出限(LOD)和定量限(LOQ)分别为 0.004 和 0.013 ppm。标准溶液和样品溶液的重复性测试表明,该方法是精确的,且在可接受的范围内。测定精度的 RSD% 为 2%。稳健性和溶液稳定性的结果也在可接受的范围内。最后,新方法在所有分析方法验证参数方面都取得了优异的结果,符合验收标准。此外,新方法的运行时间短,保留时间约为 4 分钟。
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引用次数: 0
Chemical Fingerprint Analysis and Content Determination of Horned Gallnut and Bellied Gallnut in Galla Chinensis 五倍子中角五倍子和腹五倍子的化学指纹分析和含量测定
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-31 DOI: 10.1155/2023/8849341
Xiaomei Long, Shuang Guo, Jianxing Gu, Lijun Zhang, Haipeng Liu, Yuan Fan, Weibo Wen
To establish an objective and comprehensive methodology to analyse the connections and differences between horned gallnut (HG) and bellied gallnut (BG) in Galla Chinensis (GC). The HPLC fingerprints from 15 batches of HG and 15 batches of BG were performed, and chemometric analysis including similarity analysis (SA), hierarchical clustering analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discrimination analysis (OPLS-DA) was also set up. The results showed that the similarity of all batch samples was more than 0.9. In fingerprint analysis, 8 distinct common peaks were detected, among which gallic acid (GA), 1,3,6-tri-O-galloyl-β-D-glucose (TGG), and 1,2,3,4,6-O-galloyl-D-glucose (PGG) were identified by comparing with the standard compounds. Meanwhile, samples were clearly grouped into two classifications corresponding to HG and BG. This study demonstrated that HPLC fingerprints coupled with chemometric analysis could be applied to discriminate HG and BG and evaluate the qualities of HG and BG rapidly, which provided a certain experimental basis for the selection of GC raw materials and subsequent use.
建立一种客观、全面的方法来分析五倍子(GC)中角五倍子(HG)和腹五倍子(BG)之间的联系和差异。对 15 批 HG 和 15 批 BG 进行高效液相色谱指纹图谱分析,并建立了相似性分析(SA)、层次聚类分析(HCA)、主成分分析(PCA)和正交偏最小二乘判别分析(OPLS-DA)等化学计量学分析方法。结果表明,所有批次样品的相似度均大于 0.9。在指纹图谱分析中,通过与标准化合物的比较,发现了 8 个明显的共性峰,其中包括没食子酸(GA)、1,3,6-三-O-配糖体-β-D-葡萄糖(TGG)和 1,2,3,4,6-O-配糖体-D-葡萄糖(PGG)。同时,样品被清晰地分为 HG 和 BG 两类。该研究表明,高效液相色谱指纹图谱结合化学计量分析法可用于鉴别 HG 和 BG,并快速评价 HG 和 BG 的品质,为 GC 原料的选择和后续使用提供了一定的实验依据。
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引用次数: 0
Effects of Soil Properties on Pb, Cd, and Cu Contents in Tobacco Leaves of Longyan, China, and Their Prediction Models 土壤特性对中国龙岩烟叶中铅、镉和铜含量的影响及其预测模型
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-12-28 DOI: 10.1155/2023/9216995
Wei Xi, YuanYe Ping, HaiYang Cai, Qian Tan, Chaoyang Liu, Junru Shen, YaWen Zhang
Longyan City in Fujian Province is one of China’s top-quality tobacco-producing areas and plays an essential role in local economic development. To determine the correlation between heavy metal content in tobacco leaves and soil factors, soil physical and chemical properties and heavy metal contents of lead, cadmium, and copper in tobacco leaves were measured and analyzed by the correlation regression method. The content of lead, cadmium, and copper in soil was determined using hydrochloric acid extraction-AAS and graphite furnace atomic absorption spectrometry. Inductively coupled plasma-mass spectrometry was used to determine heavy metal in tobacco leaf. The findings revealed that the average concentrations of lead, cadmium, and copper in the soil were 12.1, 0.092, and 3.88 mg/kg, respectively. In contrast, the average levels of lead, cadmium, and copper in tobacco leaves were 2.33, 4.89, and 4.35 mg/kg, respectively. The cadmium enrichment coefficient of 54.3 was higher than lead and copper, indicating a greater health risk. Soil pH value was negatively correlated with lead content in tobacco leaf, while potassium and phosphorus nutrient levels were negatively correlated with copper content. In contrast, a positive correlation was established between the presence of organic matter with cadmium content in tobacco leaves. The prediction models of lead, cadmium, and copper in tobacco leaves can be expressed by the regression equation corresponding to each heavy metal as follows: <span><svg height="14.0004pt" style="vertical-align:-5.3645pt" version="1.1" viewbox="-0.0498162 -8.6359 28.655 14.0004" width="28.655pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,0,0)"></path></g><g transform="matrix(.0091,0,0,-0.0091,7.111,3.132)"></path></g><g transform="matrix(.0091,0,0,-0.0091,12.234,3.132)"></path></g><g transform="matrix(.013,0,0,-0.013,21.024,0)"></path></g></svg><span></span><svg height="14.0004pt" style="vertical-align:-5.3645pt" version="1.1" viewbox="32.2361838 -8.6359 105.84 14.0004" width="105.84pt" xmlns="http://www.w3.org/2000/svg" xmlns:xlink="http://www.w3.org/1999/xlink"><g transform="matrix(.013,0,0,-0.013,32.286,0)"></path></g><g transform="matrix(.013,0,0,-0.013,38.526,0)"></path></g><g transform="matrix(.013,0,0,-0.013,41.49,0)"></path></g><g transform="matrix(.013,0,0,-0.013,47.731,0)"><use xlink:href="#g113-52"></use></g><g transform="matrix(.013,0,0,-0.013,56.876,0)"></path></g><g transform="matrix(.013,0,0,-0.013,67.413,0)"></path></g><g transform="matrix(.013,0,0,-0.013,73.653,0)"><use xlink:href="#g113-47"></use></g><g transform="matrix(.013,0,0,-0.013,76.617,0)"><use xlink:href="#g113-49"></use></g><g transform="matrix(.013,0,0,-0.013,82.857,0)"><use xlink:href="#g113-49"></use></g><g transform="matrix(.013,0,0,-0.013,89.097,0)"></path></g><g transform="matrix(.013,0,0,-0.013,98.243,0)"></path></g><g transform="matrix(.013,0,0,-0.013,110.954,0)"></path><
福建省龙岩市是中国优质烟叶产区之一,在当地经济发展中发挥着重要作用。为了确定烟叶中重金属含量与土壤因子的相关性,采用相关回归法测定并分析了土壤理化性质和烟叶中铅、镉、铜等重金属含量。采用盐酸萃取-原子吸收光谱法和石墨炉原子吸收光谱法测定了土壤中铅、镉和铜的含量。采用电感耦合等离子体质谱法测定了烟叶中的重金属含量。结果显示,土壤中铅、镉和铜的平均浓度分别为 12.1、0.092 和 3.88 毫克/千克。而烟叶中铅、镉和铜的平均含量分别为 2.33、4.89 和 4.35 毫克/千克。镉的富集系数为 54.3,高于铅和铜,表明对健康的风险更大。土壤 pH 值与烟叶中的铅含量呈负相关,而钾和磷营养水平与铜含量呈负相关。相反,有机物的存在与烟叶中的镉含量呈正相关。烟叶中铅、镉和铜含量的预测模型可以用各重金属对应的回归方程表示如下: (分别为( = 0.787)、( = 0.891)和( = 0.724)。上述预测模型为利用研究区域的土壤特性评估烟叶重金属风险提供了有效的预测工具。
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引用次数: 0
Facile and Sensitive Acetylene Black-Based Electrochemical Sensor for the Detection of Imatinib 简便灵敏的乙炔黑基电化学传感器检测伊马替尼
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-30 DOI: 10.1155/2023/3228470
Shun Li, Qingwu Tian, Xuanming Xu, Chao Xuan, Xiaomin Yang, Shukai Sun, Tingting Zhou
A facile and sensitive electrochemical sensor for determining imatinib (IMA) was constructed by modifying a glassy carbon electrode (GCE) with a nanocarbon material, acetylene black (AB). The electrochemical behavior of IMA on the prepared GCE/AB was studied using electrochemical techniques, namely, differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy. The direct determination of IMA by the GCE/AB sensor was accomplished using DPV under optimized conditions. The method verification showed that the oxidation peak current was proportional to the concentrations of IMA in the linear ranges of 0.01–0.5 and 0.5–4 μM, with correlation coefficients of 0.9856 and 0.9946, respectively. The limit of detection of the GCE/AB sensor was 0.15 nM. Moreover, the GCE/AB sensor showed good precision and accuracy. Finally, the GCE/AB sensor was successfully applied to determine IMA in human serum samples, and the recoveries were satisfactory.
采用纳米碳材料乙炔黑(AB)修饰玻碳电极(GCE),构建了一种简便灵敏的测定伊马替尼(IMA)的电化学传感器。采用差分脉冲伏安法(DPV)和电化学阻抗谱技术研究了IMA在制备的GCE/AB上的电化学行为。在优化条件下,采用DPV法实现了GCE/AB传感器对IMA的直接测定。方法验证表明,氧化峰电流与IMA浓度在0.01 ~ 0.5 μM和0.5 ~ 4 μM线性范围内成正比,相关系数分别为0.9856和0.9946。GCE/AB传感器的检测限为0.15 nM。GCE/AB传感器具有良好的精度和准确度。最后,GCE/AB传感器成功应用于测定人血清样品中的IMA,回收率令人满意。
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引用次数: 0
Retracted: Application of 3D Printing Technology and Porous Nano-Ceramic Decorative Sheet in Interior Landscape Design. 撤回:三维打印技术和多孔纳米陶瓷装饰板在室内景观设计中的应用。
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-29 eCollection Date: 2023-01-01 DOI: 10.1155/2023/9863810
International Journal Of Analytical Chemistry

[This retracts the article DOI: 10.1155/2022/8715211.].

[本文撤回文章 DOI:10.1155/2022/8715211.]。
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引用次数: 0
Retracted: Extraction and Dyeing Techniques of Traditional Vegetable Dyestuffs. 撤回:传统植物染料的提取和染色技术。
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-29 eCollection Date: 2023-01-01 DOI: 10.1155/2023/9849345
International Journal Of Analytical Chemistry

[This retracts the article DOI: 10.1155/2022/4173886.].

[本文撤消了文章 DOI:10.1155/2022/4173886.]。
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引用次数: 0
Retracted: Application of Calcium-Based Nanomaterials in Art Sculpture Reinforcement Technology. 撤回:钙基纳米材料在艺术雕塑加固技术中的应用。
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-29 eCollection Date: 2023-01-01 DOI: 10.1155/2023/9864120
International Journal Of Analytical Chemistry

[This retracts the article DOI: 10.1155/2022/9593268.].

[本文撤回了文章 DOI:10.1155/2022/9593268]。
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引用次数: 0
Retracted: Research on Nanoeffect of Penetration and Consolidation under Nonlinear Characteristics of Saturated Soft Clay. 撤回:饱和软粘土非线性特征下渗透与固结的纳米效应研究
IF 1.8 4区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-29 eCollection Date: 2023-01-01 DOI: 10.1155/2023/9832943
International Journal Of Analytical Chemistry

[This retracts the article DOI: 10.1155/2022/7463817.].

[此文撤消了文章 DOI:10.1155/2022/7463817.]。
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引用次数: 0
期刊
International Journal of Analytical Chemistry
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