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Separation Science Plus · 2019 ·Vol. 2 ·期 10 ·384-391 · IF 0

Rapid determination of ferulic acid in three kinds of Chinese herbs by direct analysis in real-time mass spectrometry

Zhongping Huang,Xiaoli Huang,Huijun Liu,Lili Wang,Yilei Fan,Charles Liu,Yiping Ren

A new method of direct analysis in real-time integrated with mass spectrometry was established and applied to the rapid determination of ferulic acid in Chinese herbs. Instrument parameter settings were optimized to obtain the sensitive and accurate determination of ferulic acid. At the sample introduction speed of 0.5 mm/s, high signal intensity of [M-H] − ( m/z 193) for ferulic acid was achieved in the negative ion mode by utilization of high purity helium gas at 350°C. The calibration curve was linear over the range of 5 – 100 mg/L with the correlation coefficient r = 0.9846 and relative standard deviation (n = 6) in the range of 2.0 to 6.1%. The limit of detection ( S/N = 3) and limit of quantitation ( S/N = 10) were 0.4 and 1.2 mg/L respectively. The recoveries were in the range of 90.6–114.2%. The results of direct analysis in real time-mass spectrometry were in agreement with those obtained by high performance liquid chromatography. The proposed direct analysis in real time mass spectrometry method is a simple, rapid and high-throughput approach for the determination of ferulic acid in Chinese herbs.

研究领域: 中药学 · 分析化学
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JOURNAL OF SEPARATION SCIENCE · 2017 ·Vol. 40 ·期 24 ·4857-4864 · IF 2.557

Rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves by direct analysis in real time-mass spectrometry

Zhongping Huang,Yueting Xu,Yilei Huang,Charles Liu,Kezhi Jiang,Lili Wang

A novel method based on direct analysis in real time integrated with mass spectrometry was established and applied into rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves. Instrument parameter settings were optimized to obtain the sensitive and accurate determination of ginkgolic acids. At the sample introduction speed of 0.2 mm/s, high intensity of [M–H] – ions for ginkgolic acids were observed in the negative ion mode by utilization of high-purity helium gas at 450°C. Two microliters of methanol extract of G. biloba kernels or leaves dropped on the surface of Quick-Strip module was analyzed after solvent evaporated to dryness. A series of standard solutions of ginkgolic acid 13:0 in the range of 2–50 mg/L were analyzed with a correlation coefficient r = 0.9981 and relative standard deviation ( n = 5) from 12.5 to 13.7%. The limit of detection was 0.5 mg/L. The results of direct analysis in real time-mass spectrometry were in agreement with those observed by thermochemolysis gas chromatography. The proposed method demonstrated significant potential in the application of the high-throughput screening and rapid analysis for ginkgolic acids in dietary supplements.

研究领域: 分析化学 · 植物化学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2019 · IF 2.983

Development of a novel assay of molecularly imprinted membrane by design-based gaussian pattern for vancomycin determination

Haining Yu,Ru Yao,Shengrong Shen

A molecularly imprinted membrane (MIM) with vancomycin (VCM) as a template and other related different material membranes (organic nylon microporous membranes, polyvinylidene fluoride (PVDF) membranes, polypropylene membranes) as a support respectively were synthesized by surface imprinting for the selective absorption of VCM, which can be used for pretreatment biological samples and rapid determination of VCM. The optimal ratio of template and functional monomer was 1:4, which was simulate by Gaussian, and the results showed that PVDF MIM had the best selectivity of the other three synthesized membranes to be used in the experiment. The maximum load on PVDF MIM was 23.8μg/cm 2 , and on non-molecularly imprinted membrane was 1.7μg/cm 2 . Additionally, performance of PVDF MIM, including surface structure, adsorption capacity, selective adsorption capacity, were also examined in this work. VCM in sample was enriched and separated effectively by PVDF MIM, and was quantitatively analyzed significantly by UV. The optimum eluent was 0.1 mol/L KOH aqueous solution in methanol (v/v=1/4), which desorption time was around 20 min. Also, recovery rate, precision, stability, linearity and repeatability for the novel assay were investigated respectively. The results indicated that separation and enrichment of VCM in biological samples by VCM MIM was reliable. The development of the assay, across a range of analytical and separated techniques for which MIM appeared to be the best support, was giving rise to increased interest in the determination of antibiotics as speedy assay for the blood concentration in clinical.

研究领域: 分析化学 · 药物分析 · 生物医学工程
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JOURNAL OF ANALYTICAL CHEMISTRY · 2025 ·Vol. 80 ·期 7 ·1163-1169 · IF 1.1

Synthesis of a Pb(II) Photoresponsive Probe and Its Application to the Rapid Determination of Pb(II) in Mustard Samples

Li Xichen,Lin Zhengzhong

Lead ions in food can accumulate in the human body, leading to various diseases, so it is necessary to detect the content of lead ions in food. In this paper, a new Schiff base was prepared using derivatives of isophthalic acid and salicylaldehyde as a photoresponsive probe for Pb(II) ions. The Schiff base probe had an absorption peak at 505 nm after the addition of Pb(II) ions to an acetonitrile solution. However, other inorganic ions caused only slight absorbance changes at 505 nm. Based on this, a visible light analysis method for Pb(II) ions was established. The equilibrium time of the Schiff base probe with Pb(II) ions was 5 min, with a linear range of 2.5–25 ppm. The Schiff base probe was used to detect Pb(II) ion content in mustard samples, and the recoveries were over 90%. The detection results were not significantly different from those of the standard method, indicating that the Schiff base probe can be used for the rapid determination of Pb(II) ion content in real samples.

研究领域: 分析化学 · 环境化学 · 食品安全 · 材料科学
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SENSORS AND ACTUATORS A-PHYSICAL · 2023 · IF 4.6

Quantitative determination of heavy metal Pb content in soybean oil based on microwave detection technique combined with multivariate analysis

Hui Jiang,Jinqi Chen,Jihong Deng,Xiang Zhao,Leijun Xu

This study provides a reference for rapid determination of heavy metal Pb in soybean oil by microwave detection technique. The microwave transmission coefficients of soybean oil samples with different concentrations of the heavy metal Pb were collected using a portable microwave detector made by our team. Three feature optimization methods, which were bootstrapping soft shrinkage (BOSS), competitive adaptive reweighted sampling (CARS), and variable combination population analysis (VCPA), were employed to select the features of microwave transmission coefficients after least square filtering, and partial least squares (PLS) models constructed on features selected were used to rapid determine the heavy metal Pb content in soybean oil. The results showed that the three variable optimization algorithms can screen out highly targeted features. Especially, the CARS-PLS model obtained the optimal generalization performance, and its coefficient of determination ( R P 2 RP2 ) and residual predictive deviation (RPD) were 0.9857 and 8.3838, respectively. The results reveal that it is feasible to use the microwave detection technique combined with appropriate chemometrics methods to determine the heavy metal Pb in soybean oil with high precision. This study provides a practical technique for nondestructive determination of heavy metal residues in edible oil .

CAS / MDL: 8006-64-2
研究领域: 食品科学 · 化学计量学
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RSC Advances · 2021 ·Vol. 11 ·期 47 ·29752-29761 · IF 3.361

Synthesis, characterization, and evaluation of selective molecularly imprinted polymers for the fast determination of synthetic cathinones

Hong Chen,Fangsheng Wu,Yibing Xu,Yuan Liu,Lun Song,Xiujuan Chen,Qun He,Wei Liu,Qiaoying Han,Zihua Zhang,Yun Zou,Wenbin Liu

As a kind of new psychoactive substance (NPS), synthetic cathinones have drawn great worldwide attention. In this study, molecularly imprinted polymers (MIPs), as adsorbents for the extraction and determination of 4-methyldimethcathinone (4-MDMC), were first synthesized by coprecipitation polymerization. The physicochemical analyses of MIPs were successfully performed by XRD, FTIR, FESEM and TGA techniques. Furthermore, rebinding properties of temperature and pH dependence, and selectivity and reusability tests for MIPs and non-imprinted polymers (NIPs) were performed using an ultraviolet-visible spectrometer (UV-vis). The obtained results indicate that the imprinting efficiency has strong dependence on temperature and pH, and the optimal adsorption for targets is achieved under the condition of 318 K and pH = 6.0. This means that the combination between the polymers and 4-MDMC is a strong spontaneous and endothermic process. Compared with NIPs, MIPs exhibit prominent adsorption capacity (Qe = 9.77 mg g−1, 318 K). The selectivity coefficients (k) of MIPs for 4-MDMC, methylenedioxypentedrone (βk-MBDP), 4-ethylmethcathinone (4-EMC), methoxetamine (MXE) and tetrahydrofuranylfentanyl (THF-F) were found to be 1.70, 3.49, 7.14 and 5.82, respectively. Moreover, it was found that the adsorption equilibrium was achieved within 30 min. The aim of this work is the simple synthesis of MIPs and the optimal performance of the molecular recognition of 4-MDMC. Moreover, the synthesized MIPs can be easily regenerated and repeatedly used with negligible loss of efficiency (only 9.94% loss after six times adsorption–desorption tests). Satisfying recoveries in the range of 69.3–78.9% indicate that MIPs have good applicability for analyte removal from urine samples. Ultimately, this material shows great promise for the rapid extraction and separation of synthetic cathinones, which are dissolved in the liquid for the field of criminal sciences.

CAS / MDL: 1310-58-3 7647-01-0
研究领域: 分析化学 · 法医学 · 材料科学
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 42 ·期 18 ·2957-2967 · IF 2.516

A method for rapid determination of arsenic species in vegetables using microwave-assisted extraction followed by detection with HPLC hyphenated to inductively coupled plasma-mass spectrometry

Xintong Jia,Xiaoyue Yang,Wei Zhao,Yuanan Hu,Hefa Cheng

Driven by the significant need for characterization of the chemical speciation of arsenic in food, this work developed a method for rapid determination of four common arsenic species, namely, arsenite, arsenate, monomethyl arsenic acid, and dimethyl arsenic acid, in vegetables using microwave-assisted extraction, followed by detection with high-performance liquid chromatography hyphenated to inductively coupled plasma-mass spectrometry. Initial screening results showed that microwave-assisted extraction using 1% HNO 3 exhibited the highest overall efficiencies for all arsenic species without causing significant degradation of the organic ones. With the aid of response surface methodology, the optimum conditions established for extraction of arsenic species from vegetables were: 500 mg of freeze-dried vegetable sample, extracted by closed vessel microwave-assisted extraction using 10 mL of 2% v/v HNO 3 at 90°C for 17 min. Application of the method in the analysis of 24 market vegetable samples indicates that the extraction efficiencies for total arsenic species were in the range of 91.4–106%. Arsenite and arsenate were found to be the predominant arsenic species in the vegetables, which suggests that vegetable consumption could be an important route of inorganic arsenic exposure for the population with a heavy vegetable diet in arsenic polluted regions.

研究领域: 分析化学 · 环境科学 · 食品安全
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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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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2022 ·Vol. 414 ·期 26 ·7731-7740 · IF 4.478

Enzyme-free colorimetric detection of biothiols based on the photoinduced oxidation of 3,3′,5,5′-tetramethylbenzidine

Liao Jun,Yu Zhicheng,Fu Li,Liu Jia,Jia Li

Realizing the rapid and on-site detection of biothiols in complex biological and food samples using simple assays and devices remains a major challenge. In this study, biothiols containing sulfhydryl groups were found to be able to inhibit the photo-triggered oxidation of 3,3′,5,5′-tetramethylbenzidine (TMB). Based on the discovery, using the commercially available and low-cost TMB as the chromogenic substrate, an enzyme-free colorimetric approach was developed for the rapid determination of biothiols. The method does not involve the introduction of any natural enzymes, nanoenzymes, and external oxidants. The mechanisms of the photoinduced oxidation of TMB and the detection of biothiols were proposed. Furthermore, a smartphone-based portable device integrated with test strips was constructed by the 3D printing technique. This device can simultaneously meet the requirements of the photocatalytic oxidation reaction of TMB and the detection of biothiols. The entire process only takes less than 5 min. The successful detection of cysteine in urine and milk samples demonstrates the great potential of the device in the on-site assays. Graphical abstract

CAS / MDL: 67-68-5
研究领域: 分析化学 · 生物技术 · 现场即时检测
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2014 · IF 3.107

Combination of Running-Buffer-Mediated Extraction and Polyamidoamine-Dendrimer-Assisted Capillary Electrophoresis for Rapid and Sensitive Determination of Free Fatty Acids in Edible Oils

Jingqing Wu,Ying Ge,Weidong Qin

A method was developed for determining free fatty acids in edible plant oils by incorporation of running-buffer-mediated liquid–liquid extraction and polyamidoamine-dendrimer-assisted capillary electrophoresis–capacitively coupled contactless conductivity detection. The recoveries for the extraction were in the range of 90.1% and 110.3%. Addition of dendrimer to the running buffer improved the separation of fatty acids. Under the optimized buffer conditions, i.e., 3 mM pelargonic acid, 39 mM tris(hydroxymethyl)aminomethane, 30 mM polyoxyethylene 23 lauryl ether, 35% acetonitrile, 15% 2-propanol, 2.5% 1-octanol, and 300 μM polyamidoamine generation 2 at apparent pH 8.53, the 10 model fatty acids were separated in 18 min with detection limits ranging from 0.46 to 3.28 μM. The successful determination of fatty acids in real samples suggests that the method is simple, cost-effective, and easy to operate and is suitable for scanning free fatty acid in edible plant oils.

研究领域: 分析化学 · 食品科学 · 电泳技术
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 2 ·1-8 · IF 5.479

An infrared IgG immunoassay based on the use of a nanocomposite consisting of silica coated Fe3O4 superparticles

Wang Kexin,Ding Yadan,Hong Xia,Liu Yichun

A reliable, rapid and ultrasensitive immunoassay is described for determination of immunoglobulin G (IgG). It is making use of biofunctional magnetite (Fe 3 O 4 ) superparticles coated with SiO 2 and serving as an infrared (IR) probe. The unique IR fingerprint signals originating from the transverse and longitudinal phonon modes, respectively, of the asymmetric stretching of the Si–O–Si bridges display a satisfactory resistance to optical interference from the environment. The adoption of Fe 3 O 4 superparticles instead of Fe 3 O 4 nanoparticles as the magnetic core warrants a controllable structure and a strong magnetic response. This facilitates the efficient purification of the probes and the alleviation of the interfacial resistance between the liquid-solid interfaces by using a magnet. The gold-coated substrate was used to immobilize goat-anti-human IgG. The analyte (human IgG) was incubated with the IR probes, and then captured by the substrate immobilized antibody with the assistance of an external magnetic field. The integral area of the IR absorption band between 1250 cm −1 – 900 cm −1 was chosen for quantitative assay. The limit of detection is 95 fM, which is two orders of magnitude better than that without the magnetic field. The assay time was shortened from 2 h to 1 min. High selectivity, specificity, and long-term stability of the immunoassay were achieved. The performance of the assay when analyzing blood samples confirmed the practicability of the method. Schematic presentation of the infrared (IR) immunoassay based on Fe 3 O 4 superparticle@SiO 2 nanocomposites. The assistance of an external magnetic field reduces the incubation time and improves the detection sensitivity.

CAS / MDL: 68-04-2
研究领域: 分析化学 · 纳米技术 · 生物传感器 · 医学诊断
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