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FOOD CHEMISTRY · 2014 · IF 3.259

Development of a rapid, simple and sensitive HPLC-FLD method for determination of rhodamine B in chili-containing products

Ping Qi,Zhihao Lin,Jiaxu Li,ChengLong Wang,WeiWei Meng,Hong Hong,Xuewu Zhang

In this work, a simple, rapid and sensitive analytical method for the determination of rhodamine B in chili-containing foodstuffs is described. The dye is extracted from samples with methanol and analysed without further cleanup procedure by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD). The influence of matrix fluorescent compounds (capsaicin and dihydrocapsaicin) on the analysis was overcome by the optimisation of mobile-phase composition. The limit of determination (LOD) and limit of quantification (LOQ) were 3.7 and 10   μg/kg, respectively. Validation data show a good repeatability and within-lab reproducibility with relative standard deviations <10%. The overall recoveries are in the range of 98–103% in chili powder and in the range of 87–100% in chili oil depending on the concentration of rhodamine B in foodstuffs. This method is suitable for the routine analysis of rhodamine B due to its sensitivity, simplicity, reasonable time and cost.

CAS / MDL: 404-86-4 19408-84-5
✓ 已验证 产品关联 DOI PubMed 高影响因子
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LUMINESCENCE · 2016 ·Vol. 32 ·期 1 ·4-10 · IF 1.452

Resonance Rayleigh scattering technique as a detection method for the RP-HPLC determination of local anaesthetics in human urine

Dan Liu,Jingdong Peng,Shaopu Liu,Mingqiong Zhou,Jing Zhang,Aiping Li

A highly selective and sensitive method of reversed phase high-performance liquid chromatography (RP-HPLC) coupled with resonance Rayleigh scattering (RRS) was developed for the determination of procaine, bupivacaine and tetracaine. Separation of three local anaesthetics was achieved at 35 °C on a C 18 column. The mobile phase was 30: 70 (v/v) acetonitrile/triethylamine–phosphoric acid buffer (pH 2.9) at flow rate of 0.3 mL/min. The RRS detection was conducted by taking advantage of the strong RRS enhancement of the local anaesthetics with erythrosine reaction in an acidic medium. Under optimum conditions, the limit of detection (S/N = 3) values were in the range of 2.4–11.2 ng/mL. Recoveries from spiked human urine samples were 95.8%–104.5%. The proposed method applied to the determination of local anaesthetics in human urine achieved satisfactory results. In addition, the mechanism of the reaction is fully discussed. Copyright © 2016 John Wiley & Sons, Ltd.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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MICROCHIMICA ACTA · 2017 ·Vol. 184 ·期 10 ·4099-4106 · IF 4.58

A nanocrystalline metal organic framework confined in the fibrous pores of core-shell silica particles for improved HPLC separation

Qu Qishu,Si Yang,Xuan Han,Zhang Kehua,Chen Xiaoming,Ding Yi,Feng Shaojie,Yu Han-Qing

A hybrid material was prepared from a metal-organic framework (MOF) and core-shell silica by using a kinetic controlling approach. The nanocrystalline MOF (HKUST-1) was prepared from 1,3,5-benzenetricarboxylate and copper(II) by tuning the reaction rate via the fraction of ethanol in the solvent. After the reaction rate was reduced to a certain degree, the pore surface would be well covered with Cu(II), which initiated the formation of a nanocrystalline HKUST-1. The resulting hybrid material was packed into a stainless-steel column (4.6 × 150 mm) and used as a stationary phase in high performance liquid chromatography. SiO 2 @ d SiO 2 -HKUST-1 combined the merits of the high separation performance of the core-shell particles and the unique selectivity of the HKUST-1 nanocrystals. A separation efficiency as high as almost 140,000 plates per meter was achieved for the model analyte styrene. The material was stable and exhibited a highly reproductivity. The relative standard deviations of column-to-column, intra-day, and inter-day reproducibility of the SiO 2 @ d SiO 2 -HKUST-1 packed columns for the retention time of styrene were 4.7%, 0.3%, and 0.4%, respectively. HKUST-1 nanocrystals were coated onto the porous surface of core-shell silica spheres under careful kinetic control. The resulting particles were packed into the column, and a separation performance of up to 140,000 plates per meter was achieved.

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JOURNAL OF FOOD BIOCHEMISTRY · 2016 ·Vol. 40 ·期 4 ·603-612 · IF 0.832

Antioxidant Activity and Phenolic Acids Profiles of Artemisia Selengensis Turcz Extracted with Various Methods by HPLC-QTOF-MS/MS

Lu Zhang,Zong-Cai Tu,Hui Wang,Qing-Hui Wen,Zhi-Feng Fu,Xing Xie

Effects of dynamic high pressure microfluidization (DHPM), microwave, ultrasound, maceration and high temperature, on the phenolic acids and antioxidant activity of Artemisia selengensis Turcz (AST) were investigated. Microwave exhibited the best extraction efficacy on phenolic compounds and flavonoids with the content of 40.30 μg GAE/mg Extract, and 37.75 μg RTE/mg Extract, respectively. Microwave extract (MWE) also showed the strongest DPPH· and HO· scavenging ability (IC 50 value of 0.23 and 0.50 mg/mL, respectively), and reducing power (Ab 0.3 value of 0.23 mg/mL). Quinic acid, 3 caffeoylquinic acids (CQAs), 2 coumaroylquinic acids, 4 dicaffeoylquinic acids (diCQAs) were identified as the major phenolic acids in AST using HPLC-QTOF-MS/MS, and 3-CQA (63.71 μg/mL) showed the highest content followed by 1,5-diCQA (17.91 μg/mL) and 3,5-diCQA (13.50 μg/mL). MWE had the highest 3-CQA and diCQAs. While, high temperature could promote the degradation of diCQAs, 3- and 4-caffeoyl are more liable to decompose as compared with 1- and 5-caffeoyl. Practical Application Over production of reactive oxygen species (ROS) in body will induce various chronic diseases. AST is an underutilized vegetable with many health benefits. This research indicates that AST possessed appreciating antioxidant activities and abundant phenolic acids, it is could be a potentail antioxidants resource and for prevention of chronic diseases associated with ROS. It also suggested that microwave could be a promising method for extracting the antioxidants in AST. Therefore, this research could lay a foundation for the high-value application of AST in food, health care and natural therapy industry, and provide some methodological references for the development of antioxidants in AST.

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Food Analytical Methods · 2017 ·Vol. 10 ·期 12 ·3856-3865 · IF 2.038

An Improved HPLC-FLD for Fast and Simple Detection of Ethyl Carbamate in Soy Sauce and Prediction of Precursors

Zhou Kai,Liu Yao,Li Wen-Qian,Liu Gong-Liang,Wei Na,Sun Yuan-Ming,Bai Wei-Dong,Xu Zhen-Lin

A high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method for ethyl carbamate (EC) determination in Chinese soy sauce was developed and used to predict EC precursors, and extraction, derivatization, and chromatographic conditions were optimized systematically. Under optimal conditions, the limit of detection, linear range, and recoveries were 3.91 μg/L, 12.87–274.87 μg/L, and 81.5–95.4%, respectively. The method precision was less than 8.9% (RSD) and no significant difference was found between EC determinations measured by HPLC-FLD and GC/MS. Using the proposed HPLC-FLD method, the EC contents in Chinese soy sauces ranged from not detected to 64.88 μg/L ( n  = 19). Except for one soy sauce brand, the EC contents in low-salt solid-state fermented (LSF) soy sauces were lower than those in high-salt liquid fermented (HLF) soy sauces and were mainly affected by alcohol content. Moreover, the free ornithine and total arginine contents were significantly correlated with EC content in the soy sauce products. The results of this work provide a foundation for further study of EC formation and inhibition in Chinese soy sauces.

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JOURNAL OF FOOD BIOCHEMISTRY · 2017 ·Vol. 41 ·期 6 ·e12402 · IF 1

Antioxidant activity, α-glucosidase inhibition, and phytochemical fingerprints of Anoectochilus roxburghii formula tea residues with HPLC-QTOF-MS/MS

Xing Xie,Zong-Cai Tu,Lu Zhang,Yi Zhao,Hui Wang,Zhen-Xing Wang,Nan-Hai Zhang,Bi-Zhen Zhong

This study assessed the phytochemical composition, antioxidant activities, and α-glucosidase inhibition of Anoectochilus roxburghii formula tea (ARFT) residue by comparing with that of ARFT infusion and ARFT extract. ARFT residue extract showed the maximum total phenolics, total flavonoids, and total condensed tannins content, with the values of 146.70 GAE mg/g E, 58.50 QE mg/g E, and 312.08 mg CE/g E, respectively, while ARFT infusion exhibited the lowest values. The strongest ABTS + · scavenging ability and α - glucosidase inhibition were also found in ARFT residue extract, but the best DPPH· scavenging ability was observed on the 95% ethanol extract of ARFT. Totally, 29 compounds were tentatively identified from the ARFT residue extract by using HPLC-QTOF-MS/MS, including 2 organic acids, 17 flavonoids, 4 fatty acids, 5 saponins, and 1 sugar. The results indicated that ARFT residue can be a promising source of natural antioxidants and α - glucosidase inhibitors. Practical applications Anoectochilus roxburghii formula tea (ARFT) is a popular health-promoting tea in China, but research on the bio-activities and functional constitution of ARFT and its residues is not available. This study suggested promising antioxidant and α - glucosidase inhibition of ARFT residue and revealed the presence of 29 major phytochemical compounds, which indicated that ARFT residue can be a potential resource of natural antioxidants and α - glucosidase inhibitors in food, cosmetic, and pharmaceutical industry.

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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Click chemistry-mediated stable isotope labeling combined with HPLC-MS/MS analysis for highly sensitive determination of steroid hormones

Xiao-Kang Fu,Si-Qi Han,Xiao-Bo Zhao,Jing-Yan Kang,Wei Ha,Yan-Ping Shi

Steroid hormone residues in food are a significant sources of endocrine disrupting chemicals (EDCs) that can adversely affect public health. However, the current analytical methods for determining steroid hormones using liquid chromatography-tandem mass spectrometry (LC-MS/MS) can be challenging due to the poor ionization efficiency of steroid hormones and the matrix effect of complex food samples. Herein, based on Cu(I)-catalyzed azide-alkyne cycloaddition (CuAAC) reaction and stable isotope labeling (SIL) technique, a novel pair of chemoselective probes ABI / d 5 -ABI was precisely designed and synthesized. This pair of probes comprises a H/D isotope tag, a linker, a reactive site azido group (N 3 ) and a MS tag (imidazolium salt). The probe ABI was employed to label ethynyl-containing steroid hormones in real samples and d 5 -ABI was applied to label standards, respectively, followed by mixing the two labeled samples for high performance (HP)LC-MS/MS analysis. It was found that the ionization efficiencies of target analytes were increased by 17–4532 folds after ABI labeling. More importantly, the heavy labeled samples serving as internal standards (ISs) can effectively compensate matrix effect during HPLC-MS/MS analysis. Finally, the proposed SIL-HPLC-MS/MS method was successfully used to highly sensitive determine four synthetic steroid hormones in food samples (milk, pork and egg). Furthermore, the good detection limits (0.015–0.020 ng/mL), satisfactory recoveries (75.7–122.9 %), and precisions (RSDs less than 9.2 %) were obtained. Hence, the established method not only provides new insights in designing SIL probes for determination of ethynyl-containing analytes within complex matrix, but also extends the application of CuAAC reaction in the field of food chemistry.

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MOLECULES · 2017 ·Vol. 22 ·期 11 ·1927 · IF 2.861

Chemical Fingerprint and Multicomponent Quantitative Analysis for the Quality Evaluation of Cyclocarya paliurus Leaves by HPLC–Q–TOF–MS

Yanni Cao,Shengzuo Fang,Zhiqi Yin,Xiangxiang Fu,Xulan Shang,Wanxia Yang,Huimin Yang

Cyclocarya paliurusis an edible and medicinal plant containing various bioactive components with significant health benefits. A combinative method using high-performance liquid chromatography (HPLC) fingerprint and quantitative analysis was developed and successfully applied for characterization and quality evaluation ofC. paliurusleaves collected from 18 geographical locations of China. For the fingerprint analysis, 21 common peaks were observed among the 18 samples, and these peaks were identified by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC–Q–TOF–MS), while a simultaneous quantification of 16 markers was conducted to interpret the variations of contents of these bioactive compounds among theC. paliurusleaves from different geographical locations. Quantification results showed that the contents of these sixteen investigated compounds varied greatly among the leaves from different locations. The developed new method would be a valuable reference for further study and development of this bioactive plant.Keywords:Cyclocarya paliurus;fingerprint;HPLC–Q–TOF–MS;quantitative analysis;quality evaluation

CAS / MDL: 64-18-6
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Chemosensors · 2024 ·Vol. 12 ·期 10 ·220 · IF 3.7

Fast Determination and Source Apportionment of Eight Polycyclic Aromatic Hydrocarbons in PM10 Using the Chemometric-Assisted HPLC-DAD Method

Ting Hu,Yitao Xia,You Wang,Li Lin,Rong An,Ling Xu,Xiangdong Qing

Polycyclic aromatic hydrocarbons (PAHs) are a group of organic compounds that are both toxic and hazardous to human health and ecological systems. In recent work, a novel analytical strategy based on the chemometric-assisted HPLC-DAD method was proposed for the quantification and source apportionment of eight PAHs in PM10 samples. Compared to traditional chromatographic methods, this approach does not require the purification of complex PM10 samples. Instead, it utilizes a mathematical separation method to extract analytes’ profiles from overlapping chromatographic peaks, enabling precise quantification of PAHs in PM10. Firstly, 40 PM10 samples collected in Loudi city during two sampling periods were used for analysis. Subsequently, the second-order calibration method based on alternating trilinear decomposition (ATLD) was employed to handle the three-way HPLC-DAD data. Finally, the pollution sources of PAHs were analyzed by the feature component analysis method according to the obtained relative concentration matrix. For the validation model, the average recoveries of eight PAHs were between (88.8 ± 7.6)% and (105.6 ± 7.5)%, and the root-mean-square errors of prediction ranged from 0.03 μg mL−1to 0.47 μg mL−1. The obtained limits of quantification for eight PAHs were in the range of 0.0050 μg mL−1to 0.079 μg mL−1. For actual PM10 samples, results of the feature component analysis indicated that the main source of PAHs in PM10 may be traffic emissions and coal combustion. In summary, the proposed method provided a new and rapid analysis method for the accurate determination and source apportionment of PAHs in atmospheric aerosols.

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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

Hydrolysis reaction paths and kinetics of cationic bleaching activators with different leaving groups based on LC-MS and HPLC

Fuyang Gu,Xiaoyan Wang,Jinmei Du,Yang Jiang,Dagang Miao,Yanmei Qu,Dongyan Shao,Guowei Xiao,Changhai Xu

Cationic bleaching activators can effectively achieve low-temperature bleaching in hydrogen peroxide system, but at the same time, self-hydrolysis reaction will occur to affect the low-temperature bleaching effect, and the complex hydrolysis pathways of cationic bleaching activators are still elusive. In this paper, the hydrolysis reaction pathways, mechanisms, rates and kinetics of cationic bleaching activators N-[4-(triethylaminomethyl)benzoyl]lactam chlorides (TBLCs) with different lactam leaving groups were investigated in depth by liquid chromatography-mass spectrometry (LC-MS) and high-performance liquid chromatography (HPLC). Specifically, we characterized the hydrolysis products by LC-MS and further quantified the hydrolysis products using HPLC, demonstrating that the hydrolysis can take place via two pathways, generating chain-breaking products and ring-opening products, and that both react at different rates depending on the different lactam leaving groups. Notably, the quantitative results showed that the chain-breaking products were always larger than the ring-opening products, and the chain-breaking products were ineffective for bleaching, which was the main reason for the decrease in the bleaching performance of TBLCs. The mechanism of hydrolysis is discussed and the reaction rate was determined to follow first-order kinetics using HPLC. We have successfully delineated the complete transformation pathway of the hydrolysis reaction using this method, providing valuable information for the future preparation of novel bleaching activators and the reduction of this reaction.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Magnetic surface-imprinted polymer microspheres coupled with HPLC-MS/MS for sensitive detection of amphetamine-type drugs in water

Dongqin Tan,Yue Wang,Haocheng Fan,Jing Jin,Xiaoli Sun,Dhanjai,Degao Wang

Magnetic surface imprinted polymer microspheres (Fe 3 O 4 @MIPs) were successfully synthesized via Pickering emulsion polymerization, utilizing N-Methylphenethylamine as a surrogate template for amphetamine-type drugs. Fe 3 O 4 @MIPs not only possessed excellent dispersibility and enough magnetic properties in aqueous solutions, but also displayed good selectivity towards six amphetamines, with an imprinting factor ranging from 1.8 to 2.6. The adsorption kinetics closely aligned with the pseudo-second-order model, and the adsorption efficiency exceeds 80 % for each amphetamine at equilibrium. Fe 3 O 4 @MIPs were then employed as the efficient adsorbents for the extraction of amphetamine drugs. Extraction parameters, including sample pH, the mass of adsorbent, and the type and volume of eluting solvent, were carefully optimized. In combination with the high performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC-MS/MS), a selective magnetic solid-phase extraction (MISPE) method utilizing Fe 3 O 4 @MIPs was developed for the detection of six amphetamines in water samples. The limits of detection and limits of quantitation were determined to be 5.2∼23 ng L −1 and 17∼77 ng L −1 , respectively. Recoveries for the six target drugs from lake water and sewage samples fell within the range of 87.2∼110 %. Additionally, the MISPE-HPLC-MS/MS method exhibited excellent repeatability, with a precision below 8.5 % at two spiking levels. The prepared Fe 3 O 4 @MIPs possessed the advantages of high selectivity, straightforward preparation, facile separation and good reusability, and was highly suitable for the efficient extraction of amphetamine-type substances in complex environmental water.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2024 · IF 4

Development of a rapid, accurate and efficient HPLC method for simultaneous determination of catechins and theaflavins in black tea

Yujie Ai,Qidi Wu,Haibo Yuan,Yingqin He,Yongwen Jiang,Suzhen Niu

Catechins and theaflavins , as the primary bioactive constituents of black tea, have a significant impact on its color, aroma, and flavor profile. We developed a rapid and precise method using HPLC to detect catechins and theaflavins in black tea. The method employed 0.1% formic acid-acetonitrile (phase A) and 1% formic acid-water (phase B) as mobile phases . Separation occurred on an Agilent SB-C18 column (4.6 mm × 250 mm, 5 µm), with 20 μL injection volume. Detection took place at 30 °C with a flow rate of 1 mL/min for 55 min.Quantitative determination utilized the external standard method, exhibiting high sensitivity (limit of detection: 0.19 to 5.14 μg/mL) and a strong linear correlation (R2 ≥ 0.9993) between concentration range and peak area. Precision, repeatability, and stability were excellent, with relative standard deviations (RSDs) below 5% (n = 5). The average recovery rate of standard addition ranged from 98.02% to 102.57%, with an RSD of less than 3.17% (n = 5). In summary, this straightforward, efficient, and precise approach is well-suited for both qualitative and quantitative analysis of catechins and theaflavins in tea. It overcomes the limitations of previous methods, providing a valuable tool for evaluating the quality and composition of black tea.

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