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BIOLOGICAL TRACE ELEMENT RESEARCH · 2024 · IF 3.4

Establishment and Validation of Sandell-Kolthoff Method for Saliva Iodine Determination

Su Yue,Li Ming,Xie Honglei,Hou Xin,Zhao Meng,Li Jia,Pan Haowen,Zhang Zexu,Yue Zongyu,Che Wenjing,Liu Lanchun,Cao Jiasen,Liu Peng

Saliva iodine is a useful biochemical marker for evaluating iodine status and controlling iodine-related diseases. This study aims to establish and validate a simple, reliable, and low-cost Sandell-Kolthoff (S-K) method for the determination of iodine in saliva. The method was established by considering the digestion solution type, concentration, dosage, digestion time and temperature, the volume of saliva samples, glass tube size, dosage of arsenious acid solution and ammonium ceric sulfate solution, and warm bath time. Then, the effectiveness of the method was examined by the linearity of the standard curve, detection limit, precision, and accuracy. The 1.5 mL 1 Mol/L ammonium persulfate solution at 100 °C for 90 min, the 200 μL saliva sample, glass tubes of 15 mm × 120 mm, 2.5 mL arsenious acid solution, 0.3 mL ammonium ceric sulfate solution, and 15 min for warm bath was selected to determine saliva iodine. In terms of validation of the S-K method, the linearity method has the linear range of the standard curve from 0 to 300 μg/L and the coefficient of determination ≥ 0.999; the detection limit, when the volume of saliva samples was 0.2 mL, was 4.6 μg/L; for precision, the relative standard deviation was from 0.3 to 2.8%; and for accuracy, the total recovery rate ranged from 92.8 to 107.0%. This S-K method is easy to operate, has good precision and accuracy, and can be used as a method to determine saliva iodine. It has great potential practical value in disease prevention, clinical auxiliary diagnosis, and experimental research.

研究领域: 医学检验 · 营养学
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JOURNAL OF CLINICAL LABORATORY ANALYSIS · 2018 ·Vol. 32 ·期 6 ·e22426 · IF 1.303

Performance evaluation of a chemiluminescence microparticle immunoassay for CK-MB

Zhi-yuan Lin,Yi-zhen Fang,Hong-wei Jin,Hua-yue Lin,Zhang Dai,Qing Luo,Hong-wei Li,Yan-ling Lin,Shui-zhen Huang,Lei Gao,Fei-hai Xu,Zhong-ying Zhang

Background To verify and evaluate the performance characteristics of a creatine kinase phosphokinase isoenzymes MB (CK-MB) assay kit, which produced by Xiamen Innodx Biotech Co. Ltd. Methods Evaluation was carried out according to “Guidelines for principle of analysis performance evaluation of in vitro diagnostic reagent.” The performance parameters included detection limit, linearity range, reportable range, recovery test, precision verification, interference test, cross-reactivity, matrix effect, and method comparison. Results The detection limit was 0.1 ng/mL. The assay had clinical linearity over range of 0.1 ng/mL-500 ng/mL. Reportable range was from 0.1 ng/mL to 1000 ng/mL. The average percent of recovery was 99.66%. The coefficient of variation (CV) for within-run and between-run of low CK-MB sample was 5.55% and 6.16%, respectively. As for high-level sample, it was 7.88% and 7.80%. In medical decision level, the relative deviation (Bias) of all interference tests was lower than 15%. When the sample had mild-hemolysis; hemoglobin ≤15 g/L; triglyceride ≤17 mmol/L; bilirubin ≤427.5 μmol/L; rheumatoid factor ≤206U/mL, there was no significant interference to be found. Moreover, assay kit had no cross-reaction with CK-MM and CK-BB. At last, total diagnostic accuracy of kit was 93.24%, when compared with refer kit. Conclusion Overall the results of the verification study indicated the performance of kit is met the requirements of the clinical test.

CAS / MDL: 635-65-4
研究领域: 医学检验 · 生物化学
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JOURNAL OF CHROMATOGRAPHIC SCIENCE · 2024 · IF 1.5

Development and Validation of a New High-Performance Liquid Chromatography-Ultraviolet Assay for Quantification of Mitoxantrone in Plasma of BALB/c-nu Mice

Tao Yanru,Zhao Hua,Xiang Yujie,Li Jin,Li Yanting,Hu Jiangling,Wang Hongmei,Jiang Xinhui

The concentration of mitoxantrone in the blood of mice was determined by a high-performance liquid chromatography-ultraviolet method with aloe-emodin as the internal standard. The separation was performed on a Hypersil BDS2 column (4.6 × 250 mm, 5 μm) as the analytical column, the mobile Phase A was acetonitrile, and B was 20-mM potassium dihydrogen phosphate (adding 1% triethylamine and adjusting the pH to 2.8 with phosphoric acid) and 4.6-mM sodium octyl sulfonate. The flow rate was 1.0 mL·min−1, the detection wavelength was 243 nm, the column temperature is 25 ± 5°C and the injection amount was 20 μL. Finally, the linear range of mitoxantrone was 5–200 μg·mL−1, and the correlation coefficient was r = 0.9999. The recovery rate of the method was 91.93–105.5%, and the extraction recovery rate was 91.45–105.5%. The intraday precision and interday precision were <3.29% (limit of detection = 0.3 μg·mL−1). The HPLC method established in this paper was simple, rapid, sensitive and accurate, and can be used to determine the content of mitoxantrone in mouse plasma after tail vein injection.

CAS / MDL: 481-72-1 65271-80-9
研究领域: 药理学 · 分析化学 · 生物化学
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Analytical Methods · 2014 ·Vol. 6 ·期 20 ·8129-8135 · IF 1.938

Analysis of Sudan dyes in lipstick samples by cloud-point extraction and high-performance liquid chromatography

Jinjiao Shi,Ligang Chen

A sensitive and simple method for high-performance liquid chromatography (HPLC) determination of Sudan dyes in lipstick samples after preconcentration by cloud point extraction (CPE) has been developed. The nonionic surfactant Triton X-114 was chosen as the extraction medium. Various experimental conditions were investigated to optimize the extraction and preconcentration process. Under optimum conditions, 3% Triton X-114 (v/v), ultrasonication for 20 min, pH 7, the satisfied recoveries of Sudan dyes were obtained. For the preconcentration of Sudan dyes by cloud point extraction, the solution was incubated in a thermostatic water bath at 60 °C for 10 min, and 22.5% sodium chloride (m/v) was added to the solution to facilitate the phase separation and increase the preconcentration factor. The limits of detection for the analytes are 0.11, 0.10, 0.07 and 0.08 μg g−1, respectively. The intra-day and inter-day precisions of four Sudan dyes are in the range of 4.6–6.4% and 4.4–6.7%, respectively. The recoveries of four Sudan dyes are 89.3%, 90.3%, 91.8% and 92.0%, respectively. The results demonstrate that this method is simple, rapid, sensitive and low cost. Moreover, it does not require the large consumption of organic solvents and is a non-toxic and eco-friendly method.

研究领域: 分析化学 · 化妆品科学 · 环境化学
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ACS Omega · 2025 · IF 4.3

Optimization and Validation of an HPLC Method for the Analysis of Carvedilol and Impurities

Lijuan Yuan,Weiguo Liu,Shengshuo Zhang,Lihong Huang,Jiangmin Cheng,Lanxiang He,Hangyu Zhao,Yonghua Yu

In this study, a liquid chromatography method was developed and validated for the accurate determination of carvedilol content while minimizing interference from impurity C and N-formyl carvedilol and allowing precise impurity analysis. The reliability of the method was verified through key parameters such as linearity, precision, accuracy, and stability, ensuring robust performance in the detection and quantification of carvedilol and related impurities. And, the method was tested under varying conditions, including changes in the flow rate, initial column temperature, and mobile phase pH. The results showed that the method demonstrated excellent linearity, with R2 values consistently above 0.999 for all analytes. Precision tests yielded RSD% values below 2.0%, confirming the method’s repeatability. Accuracy assessments revealed recovery rates ranging from 96.5% to 101%, while stability studies indicated minimal variation in peak areas and impurity content over extended time periods. These results confirm the method’s reliability for accurate quantification and impurity analysis in pharmaceutical samples.

CAS / MDL: 7664-38-2
研究领域: 药物分析 · 药学 · 分析化学 · 药物质量控制 · 药物代谢 · 色谱技术
✓ 已验证 产品关联 DOI PubMed 高影响因子
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SN Applied Sciences · 2019 ·Vol. 2 ·期 1 ·1-11 · IF 0

A modified QuEChERS/GC–MS for simultaneous determination of 16 pesticide adjuvant residues in fruits and vegetables

Li Genrong,Yu Wenqin,Xiao Zhaojing,Long Mei,Tong Lanyan,Qiu Yue

A rapid, sensitive, and practical QuEChERS method coupled with gas chromatography–mass spectrometry was developed for the simultaneous determination of 16 chemical adjuvant residues in samples of fruits (apple, nectarine, grape) and vegetables (tomato, cucumber, spinach). All target compounds were separated in less than 16 min. Samples were extracted with acetonitrile, and the types of extraction salt and cleanup sorbent were optimized. The optimized method was validated by evaluating the linearity, accuracy, precision, and matrix effect. The recoveries of the 16 pesticides adjuvants ranged from 61.2 to 116.3% with relative standard deviations lower than 11.6%. Limits of detection ranged from 0.21 to 3.02 μg/kg, and limits of quantification ranged from 0.71 to 10.07 μg/kg. Finally, the developed method was successfully employed to identify and quantify pesticide adjuvant residues in the analysis of 30 real fruit and vegetable samples.

研究领域: 分析化学 · 食品科学 · 环境科学
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Analytical Methods · 2021 ·Vol. 13 ·期 42 ·5075-5084 · IF 2.896

Rapid determination of sulfamethoxazole and trimethoprim illegally added to health products using excitation–emission matrix fluorescence coupled with the second-order calibration method

Lu-Zhu Chen,Hai-Long Wu,Wan-Jun Long,Tong Wang,Gao-Yan Tong,Ru-Qin Yu

In this work, a simple and fast analytical method based on a self-weighted alternating trilinear decomposition (SWATLD) algorithm coupled with excitation–emission matrix (EEM) fluorescence was developed for the simultaneous determination of sulfamethoxazole (SMZ) and trimethoprim (TMP) illegally added to health products. With the second-order advantage, the proposed method obtained satisfactory results in the presence of peak overlap and unknown interferences. The analysis time for a single sample is only 0.8 minutes. The average spiked recoveries of SMZ and TMP in three health product spiked samples were in the range of 91.0–106.2% and 86.8–107.8%, respectively. The relative standard deviations (RSDs) were lower than 8.6%. In addition, verification parameters including sensitivity (SEN), selectivity (SEL), the limit of detection (LOD), the limit of quantification (LOQ), intra-day precision, and inter-day precision were calculated, and the results show that the proposed method is feasible. The quantitative results of the proposed method were further confirmed by the LC-MS/MS method, which proved that the proposed method was efficient and green for drug-abuse monitoring of SMZ and TMP in health products.

CAS / MDL: 723-46-6 738-70-5
研究领域: 分析化学 · 药物分析 · 食品安全
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BIOMEDICAL CHROMATOGRAPHY · 2025 ·Vol. 39 ·期 10 ·e70136 · IF 1.7

Development of Mobile-Phase Buffers and Evaluation of Analytical Performance for HbA1c Assays

Yiyao Zhang,Guangyun Zhang,Fen Yang,Zhikang Zou

Hemoglobin A 1c (HbA 1c ) plays a role in the diagnosis and assessment of glycemic control in patients with diabetes. However, few studies have focused on the preparation methods and analytical performance evaluation of different formulations of mobile-phase buffers for HbA 1c assays. In this study, mobile-phase buffers of new formulations were prepared for the measurement of HbA 1c . Following the Clinical and Laboratory Standards Institute (CLSI) guidelines, the analytical performance of newly developed mobile-phase buffers was evaluated. The CVs of the intra- and inter-assay precision were less than 0.94%, the RDs of accuracy were less than ± 3.00%, and the carryover was 0.00%. The measured HbA 1c values were linear from 4.50% to 16.80% (26.00–160.00 mmol/mol). A comparison of newly developed and commercial mobile-phase buffers revealed that the Pearson regression equation was Y = 0.9862 x + 0.0888 ( R 2 = 0.9990), and the Bland–Altman mean difference between the two mobile-phase buffers was −0.02833% (95% CI: −0.1853% to 0.1278%). The chromatography column had a lifetime of over 7000 tests. The reference interval was 4.30%–6.30% (23.00–45.00 mmol/mol). Stability was acceptable within 24 months. The newly developed mobile-phase buffers demonstrated good analytical performance (i.e., precision, linearity, accuracy, carryover, reference interval, the number of chromatography column runs, and stability).

研究领域: 临床化学 · 糖尿病诊断 · 分析方法验证 · 色谱分析
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CARBOHYDRATE POLYMERS · 2024 · IF 10.7

A novel method to quantify chitosan in aqueous solutions by ultrahigh-performance liquid chromatography–tandem mass spectrometry

Ting Xue,Lei Zhou,Fanjun Wang,Zhuang Tian,Nanxi Li,Tong Ye,Ruolin Hao,Lei Yang,Ruolan Gu,Hui Gan,Zhuona Wu,Xiaoxia Zhu,Shuchen Liu,Yunbo Sun,Guifang Dou,Zhiyun Meng

In this study, a novel and accurate quantitative analysis method for the direct determination of chitosan (CS) in aqueous solutions using ultrahigh-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) is presented. By detecting the mass spectrum response intensity of a series of CS characteristic ion pairs , the sample concentration (abscissa) was linearly fitted with the total ion current (TIC) response intensity of its characteristic ion pairs (ordinate). A reliable standard curve was derived for quantifying CS in the range of 125–4000 ng/mL. Under the detection conditions, this CS quantification method yielded acceptable specificity (no interference peak), linearity (with correlation coefficient (r 2 ) values >0.999), precision (acceptable limit RSD r  < 3 %, RSD R  < 6 %), accuracy (RE within the acceptable limits of ±5 %), and stability (acceptable limit RE within ±5 %, RSD r  < 3 %). Moreover, the applicability of measurement was verified when a series of substrates did not interact with CS in the solution. Results have verified the applicability of this method for determining CS content in different composites. This study provides a method for determining CS content with significant practical value and economic benefit.

研究领域: 分析化学 · 药物分析 · 生物技术
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RSC Advances · 2017 ·Vol. 7 ·期 89 ·56528-56536 · IF 3.108

Freezing temperature controlled deep eutectic solvent dispersive liquid–liquid microextraction based on solidification of floating organic droplets for rapid determination of benzoylureas residual in water samples with assistance of metallic salt

Miyi Yang,Kun Hong,Xiaoqiang Li,Fangji Ge,Yuqing Tang

An efficient and novel salt-assisted deep eutectic solvent (DES) dispersive liquid–liquid microextraction based on solidification of floating organic droplets combined with high performance liquid chromatography was developed for extraction and determination of four benzoylureas (BUs) in water samples. In this method, a hydrophobic deep eutectic solvent (DES) used as extractant was dissolved in a dispersive-demulsified solvent containing FeCl3. The influence of main factors on the efficiency of this procedure was investigated by one-factor experimental design and central composite design (CCD) successively. Under optimal conditions, the proposed method manifest good recoveries in the range of 82.36–93.82% and high precision (relative standard deviations below 5%). The enrichment factors for the analytes changed from 91 to 97. The limits of detection varied from 0.11 to 0.35 μg L−1 with the linear coefficients greater than 0.999. The method is successfully applied to determine the BUs in different water samples, which proved the potential use of this method in real samples.

研究领域: 分析化学 · 环境科学 · 化工
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MOLECULES · 2022 ·Vol. 27 ·期 15 ·4689 · IF 4.927

Evaluation of Water Ammonium Ion Test Kit and Its Feasibility for the Analysis of Protein in Food

Dan Wu,Qile Xia,Jianfeng Zhou,Xingqian Ye

The traditional method for the determination of protein in food needs the operations of digestion, distillation, absorption, and titration; therefore, it is complicated and time-consuming and requires professional personnel. Is there a more convenient and faster detection method that can directly determine the ammonium ions in protein digestion solution to obtain the protein content of food and avoid the distillation–absorption–titration process? The feasibility of water ammonium ion test kits for food protein rapid detection was discussed here. After digestion, the protein in food transforms into ammonium ions in the digestion solution. Because of the variety of food, there are many different inorganic ions left in the food digestion solution, and at the same time, digestion agents are added in the digestion process and become potential interference factors in ammonium determination. Therefore, the detection accuracy of ammonium test kits needs to be evaluated first, including their anti-interference ability. The standard curve of ammonium was established by the test kit. When the ammonium concentration was 0.00–2.50 mg/L, the absorbance at 620 nm was linearly related to the ammonium concentration, the determination coefficient R2was 0.9995, and the detection limit of this method was 0.01 mg/L. The influences of temperature, pH value, and reaction time on the test kit method were discussed. The precision was 0.90–3.33%; the repeatability was 1.71–4.86%; and the recovery rate of tap water, river water, and sea water was controlled within 90–103%. The anti-interference ability of the evaluated test kit was better than that of the national standard detection method. The test kit, combined with sample pretreatment and protein conversion formula, was used to detect protein in different types of food (milk powder, rice flour, wheat flour, soy, banana, milk, fish food, chicken food, and dog food). The results showed that there were no significant differences (ρ > 0.05) between the national method and the test kit method. The ammonium ion test kit method shortened the determination time and had higher sensitivity, showing its potential for the rapid determination of food protein.Keywords:ammonium ion test kit;protein;rapid determination

CAS / MDL: 7440-38-2
研究领域: 食品科学 · 分析化学 · 生物技术
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Journal of Food Measurement and Characterization · 2023 · IF 3.4

Optimization and validation of folate extraction from Moringa oleifera leaves powder

Du Huan,Li Tao,Xue Qiaoli,Tian Yang,Hu Yongjin

Moringa oleifera leaves are potentially benign sources of natural folates, thus a reliable folate extraction protocol is necessary, which directly affects the accuracy of subsequent determination of total folates or various folate derivatives. With this aim, process variables including antioxidants, extraction buffer pH, Moringa oleifera leaves powder (MOLP)/extraction buffer ratio, heating extraction time, amounts of α- amylase, protease and rat serum, and also incubation time of rat serum were investigated and optimized by response surface methodology (RSM). It is interesting that no positive influence of α- amylase or protease solution was observed in this study, consequently a single-enzyme treatment was used. An average folate level of 1190.06 µg/100 g dry matter was achieved by microbial assay under the optimized conditions of extraction buffer pH 7.0, MOLP/extraction buffer ratio 1:24 (g/mL), rat serum 350 µL, digest time 2.0 h, in good agreement with the value predicted by quadratic model. In addition, the validity of protocol established in this study was confirmed. The intra-day precision (relative standard deviation) varied between 1.42% with 1.84%, inter-day precision varied in the range of 1.34–2.25%. The average recoveries were in the range of 101.56–103.27%. Besides, the matrix effects ranged from 101.41 to 103.34%. The protocol could provide a reference to fairly evaluate folates in Moringa oleifera leaves from diverse sources, and even in other leafy plants. Meanwhile, Moringa oleifera leaves with high folate level seem to have tremendous potential to increase nutritional value of foods as well as to enhance regional economies.

研究领域: 食品科学 · 营养学 · 分析化学 · 植物科学
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