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1.
Sensors (Basel) ; 24(9)2024 Apr 30.
Article in English | MEDLINE | ID: mdl-38732964

ABSTRACT

Motion object detection (MOD) with freely moving cameras is a challenging task in computer vision. To extract moving objects, most studies have focused on the difference in motion features between foreground and background, which works well for dynamic scenes with relatively regular movements and variations. However, abrupt illumination changes and occlusions often occur in real-world scenes, and the camera may also pan, tilt, rotate, and jitter, etc., resulting in local irregular variations and global discontinuities in motion features. Such complex and changing scenes bring great difficulty in detecting moving objects. To solve this problem, this paper proposes a new MOD method that effectively leverages local and global visual information for foreground/background segmentation. Specifically, on the global side, to support a wider range of camera motion, the relative inter-frame transformations are optimized to absolute transformations referenced to intermediate frames in a global form after enriching the inter-frame matching pairs. The global transformation is fine-tuned using the spatial transformer network (STN). On the local side, to address the problem of dynamic background scenes, foreground object detection is optimized by utilizing the pixel differences between the current frame and the local background model, as well as the consistency of local spatial variations. Then, the spatial information is combined using optical flow segmentation methods, enhancing the precision of the object information. The experimental results show that our method achieves a detection accuracy improvement of over 1.5% compared with the state-of-the-art methods on the datasets of CDNET2014, FBMS-59, and CBD. It demonstrates significant effectiveness in challenging scenarios such as shadows, abrupt changes in illumination, camera jitter, occlusion, and moving backgrounds.

2.
J Hazard Mater ; 465: 133104, 2024 Mar 05.
Article in English | MEDLINE | ID: mdl-38071774

ABSTRACT

Ochratoxin A (OTA), a mycotoxin found in various food items, possesses significant health risks due to its carcinogenic and toxic properties. Thus, detecting OTA is crucial to ensure food safety. Among the reported analytical methods, there has yet to be one that achieves fast, selective, and portable detection of OTA. In this study, we explore a novel supramolecular sensor, DOCE@ALB, utilizing human serum albumin as the host and a flavonoid fluorescent indicator as the guest. On the basis of indicator displacement assay, this sensor boasts an ultra-fast response time of just 5 s, high sensitivity with a limit of detection at 0.39 ppb, exceptional selectivity, and a noticeable ratiometric fluorescence response to OTA. This discernible color change and portability of the sensor make it suitable for on-site OTA detection in real food samples, including flour, beer, and wine, simply using a smartphone. In comparison to previously reported methods, our approach has showcased notable advantages in both response time and portability, addressing a critical need for food safety and regulatory compliance.


Subject(s)
Aptamers, Nucleotide , Biosensing Techniques , Mycotoxins , Ochratoxins , Humans , Food Contamination/analysis , Ochratoxins/analysis , Mycotoxins/analysis , Fluorescent Dyes , Limit of Detection , Biosensing Techniques/methods
3.
Bioact Mater ; 33: 497-505, 2024 Mar.
Article in English | MEDLINE | ID: mdl-38145214

ABSTRACT

High levels of cell-free DNA (cfDNA) induce psoriasis. Currently, the treatment of psoriasis has the disadvantages of penetration difficulty, suppression of normal immunity, and skin irritation. In this study, biguanide chitosan microneedles (BGC-MNs) were prepared to treat psoriasis by removing cfDNA from the dermis through the skin barrier. The effects of chitosan with different bisguanidine contents on DNA-binding capacity, biocompatibility, and inflammation inhibition were compared, revealing that chitosan containing 20% bisguanidine (BGC2) was found to have the best overall performance. In vitro, BGC2 effectively cleared cfDNA and inhibited the production of inflammatory factors. BGC-MN made from BGC2 had good mechanical and solubility properties. In vivo, BGC-MNs cleared cfDNA, reduced the level of inflammatory factors in the dermis, and exerted a good therapeutic effect on mice with psoriasis. These results suggested that BGC-MNs provided a new approach to treating psoriasis in terms of scavenging cfDNA and exerting anti-inflammatory effects.

4.
Plants (Basel) ; 12(17)2023 Aug 23.
Article in English | MEDLINE | ID: mdl-37687279

ABSTRACT

The detection algorithm of the apple-picking robot contains a complex network structure and huge parameter volume, which seriously limits the inference speed. To enable automatic apple picking in complex unstructured environments based on embedded platforms, we propose a lightweight YOLOv5-CS model for apple detection based on YOLOv5n. Firstly, we introduced the lightweight C3-light module to replace C3 to enhance the extraction of spatial features and boots the running speed. Then, we incorporated SimAM, a parameter-free attention module, into the neck layer to improve the model's accuracy. The results showed that the size and inference speed of YOLOv5-CS were 6.25 MB and 0.014 s, which were 45 and 1.2 times that of the YOLOv5n model, respectively. The number of floating-point operations (FLOPs) were reduced by 15.56%, and the average precision (AP) reached 99.1%. Finally, we conducted extensive experiments, and the results showed that the YOLOv5-CS outperformed mainstream networks in terms of AP, speed, and model size. Thus, our real-time YOLOv5-CS model detects apples in complex orchard environments efficiently and provides technical support for visual recognition systems for intelligent apple-picking devices.

5.
Molecules ; 28(9)2023 May 02.
Article in English | MEDLINE | ID: mdl-37175267

ABSTRACT

Cadmium sulfide nanoparticles (CdS NPs) have been employed in various fields of nanobiotechnology due to their proven biomedical properties. They are unique in their properties due to their size and shape, and they are popular in the area of biosensors, bioimaging, and antibacterial and anticancer applications. Most CdS NPs are generally synthesized through chemical, physical, or biological methods. Among these methods, biogenic synthesis has attracted more attention due to its high efficiency, environmental friendliness, and biocompatibility features. The green approach was found to be superior to other methods in terms of maintaining the structural characteristics needed for optimal biomedical applications. The size and coating components of CdS NPs play a crucial role in their biomedical activities, such as anticancer, antibacterial, bioimaging, and biosensing applications. CdS NPs have gained significant interest in bioimaging due to their desirable properties, including good dispersion, cell integrity preservation, and efficient light scattering. Despite these, further studies are necessary, particularly in vivo studies to reduce NPs' toxicity. This review discusses the different methods of synthesis, how CdS NPs are characterized, and their applications in the biomedical field.


Subject(s)
Cadmium Compounds , Nanoparticles , Nanoparticles/chemistry , Cadmium Compounds/chemistry , Sulfides/chemistry , Anti-Bacterial Agents/chemistry
6.
Plants (Basel) ; 12(9)2023 May 01.
Article in English | MEDLINE | ID: mdl-37176925

ABSTRACT

Semantic segmentation of 3D point clouds has played an important role in the field of plant phenotyping in recent years. However, existing methods need to down-sample the point cloud to a relatively small size when processing large-scale plant point clouds, which contain more than hundreds of thousands of points, which fails to take full advantage of the high-resolution of advanced scanning devices. To address this issue, we propose a feature-fusion-based method called FF-Net, which consists of two branches, namely the voxel-branch and the point-branch. In particular, the voxel-branch partitions a point cloud into voxels and then employs sparse 3D convolution to learn the context features, and the point-branch learns the point features within a voxel to preserve the detailed point information. Finally, an attention-based module was designed to fuse the two branch features to produce the final segmentation. We conducted extensive experiments on two large plant point clouds (maize and tomato), and the results showed that our method outperformed three commonly used models on both datasets and achieved the best mIoU of 80.95% on the maize dataset and 86.65% on the tomato dataset. Extensive cross-validation experiments were performed to evaluate the generalization ability of the models, and our method achieved promising segmentation results. In addition, the drawbacks of the proposed method were analyzed, and the directions for future works are given.

7.
J Mater Chem B ; 11(18): 4121-4130, 2023 05 10.
Article in English | MEDLINE | ID: mdl-37114454

ABSTRACT

The survivin gene, highly expressed in most cancer cells, is closely associated with inhibiting apoptosis. Therefore, gene editing for the survivin gene has great potential in tumor therapy. However, it is difficult for plasmid DNA (pDNA) to be taken up directly by cells, and thus the construction of gene vectors is a key step for successful gene editing. Ethanolamine-functionalized polyglycidyl methacrylate (PGEA) has been proved to facilitate the transfection of pDNA into cells in both in vivo and in vitro experiments. However, PGEA does not specifically recognize tumor cells. Some tumor cells express more mannose receptor (MR) than healthy cells. To achieve efficient target and transfection, we designed mannose-functionalized four-arm PGEA cationic polymers (P(GEA-co-ManMA), GM) with different molecular weights. GM was combined with pCas9-survivin. The mannose unit of GM/pCas9-survivin was identified by MR to selectively enter lung cancer cells. In vitro experiments showed that GM not only had excellent biocompatibility, gene transfection performance, and targeted ability, but also significantly inhibited the proliferation of tumor cells when used in combination with pCas9-survivin. At the same time, we also studied the relationship between the molecular weight and therapeutic effect.


Subject(s)
Lung Neoplasms , Mannose , Humans , Survivin , CRISPR-Cas Systems/genetics , DNA , Lung Neoplasms/genetics , Lung Neoplasms/therapy
8.
Adv Healthc Mater ; 12(23): e2300484, 2023 09.
Article in English | MEDLINE | ID: mdl-37036385

ABSTRACT

A novel class of agents is developed based on the core engineering of open-shelled organic mixed-valence (MV) systems, which enable tunable absorption and emission across the near infrared (NIR)-I to III biowindow (700-1850 nm) by adjusting the number of central nitrogen oxidation sites and the length of the conjugated bridge. Organic mixed-valence (MV) systems are synthesized through a one-step partial chemical oxidation of starburst oligoarylamines, with varying nitrogen oxidation sites and conjugated bridge lengths, including tris(4-[diethylamino]phenyl)aminen+ (T4EPAn + ), N,N,N',N'-tetrakis(4-[diisobutylamino]phenyl)-1,4-phenylenediaminen+ (TPDAn + ), and N,N,N',N'-tetrakis(4-methoxyphenyl)benzidinen+ (TMPBn + ). The absorption wavelength of the MV systems redshifted clearly as the number of central nitrogen oxidation sites increased or the conjugated bridge length is prolonged. T4EPAn + with one central nitrogen oxidation site exhibits fluorescence emission in the range of 900-1400 nm, while TPDAn + with two central nitrogen oxidation sites demonstrate strong heat generation capabilities. Additionally, the absorption peak of TMPBn + with a biphenyl conjugated bridge reaches up to 1610 nm. Especially, these MV systems are highly stable for biological applications due to their high steric hindrance and hyperconjugation effect. These characteristics make MV systems promising candidates for constructing NIR-I/II/III emitters and photothermal agents, representing a significant advance toward developing the next generation of NIR-I to III agents.


Subject(s)
Engineering , Nitrogen , Oxidation-Reduction
9.
Polymers (Basel) ; 15(5)2023 Feb 25.
Article in English | MEDLINE | ID: mdl-36904404

ABSTRACT

Self-assembly is a growth mechanism in nature to apply local interactions forming a minimum energy structure. Currently, self-assembled materials are considered for biomedical applications due to their pleasant features, including scalability, versatility, simplicity, and inexpensiveness. Self-assembled peptides can be applied to design and fabricate different structures, such as micelles, hydrogels, and vesicles, by diverse physical interactions between specific building blocks. Among them, bioactivity, biocompatibility, and biodegradability of peptide hydrogels have introduced them as versatile platforms in biomedical applications, such as drug delivery, tissue engineering, biosensing, and treating different diseases. Moreover, peptides are capable of mimicking the microenvironment of natural tissues and responding to internal and external stimuli for triggered drug release. In the current review, the unique characteristics of peptide hydrogels and recent advances in their design, fabrication, as well as chemical, physical, and biological properties are presented. Additionally, recent developments of these biomaterials are discussed with a particular focus on their biomedical applications in targeted drug delivery and gene delivery, stem cell therapy, cancer therapy and immune regulation, bioimaging, and regenerative medicine.

10.
Environ Pollut ; 263(Pt B): 114389, 2020 Aug.
Article in English | MEDLINE | ID: mdl-32220691

ABSTRACT

The present work reported a high-throughput strategy for the analysis of 21 perfluorinated compounds (PFCs) in drinking water, tap water, river water and plant effluent from southern China by supramolecular solvent (SUPARS) vortex-mixed microextraction combined with high performance liquid chromatography-Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS). The SUPRAS without heating assistance is less solvent-consumption, meeting the requirements for green environmental protection and sustainable development. Parameters in the microextraction such as volume of dodecanol and tetrahydrofuran (THF), vortexing extraction and centrifugation time, salt concentration were investigated. The optimal extraction conditions were 250 µL of undecanol, 1.0 mL of THF and 20.0% (w/v, 4 g) NaCl. Under the optimum conditions, method limit of detection and method limit of quantitation in the ranges of 0.01-0.08 µg/L and 0.03-0.25 µg/L, good recoveries (72.5-117.8%) and intra-day precision (1.1-11.2%, n = 6), high enrichment factors (48-78) were obtained. The developed method was successfully applied for analysis of PFCs in 13 drinking water, tap water, river water and plant effluent samples collected from southern China. Perfluorobutane sulfonic acid was detected in one river water with concentration of 0.48 µg/L and 1H,1H,2H,2H-Perfluorooctane sulfonic acid was detected in one river water and two plant effluent samples with concentrations in the range of 0.14-0.67 µg/L.


Subject(s)
Drinking Water/analysis , Liquid Phase Microextraction , Water Pollutants, Chemical/analysis , China , Chromatography, High Pressure Liquid , Rivers , Solvents
11.
Molecules ; 24(23)2019 Nov 21.
Article in English | MEDLINE | ID: mdl-31766469

ABSTRACT

Nowadays, the analysis of the multi-components in Chinese patent medicine prescriptions is being paid more attention. Therefore, in this study for the first time, a simple, rapid ultrahigh performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS) method was established for simultaneous determination of 18 active compounds in a Chinese patent medicine of Hu Gan tablets (HGT) from different pharmaceutical factories in China. This task has met great emerging challenges from not only structural complexities and similarities but also co-occurrence of water-soluble and fat-soluble components in HGT. UPLC-ESI-MS/MS was put forward to solve the problems. It was operated in both positive and negative mode using multiple reaction monitoring (MRM). The mobile phase was 0.1% formic acid in water (A) -0.1% formic acid in acetonitrile (B) with linear gradient elution at a flow rate of 0.2 mL/min, run for a total of 12.0 min. The optimized method used provided short analysis time and good linearity (R2 > 0.99), and intra- and inter-day precision (relative standard deviation (RSD) < 4.00%) with good accuracy (94.89-110.03%) and recovery (70.00-126.09%). The results indicate the method could be practically used for quality guarantee of HGT and might also be useful for further studies.


Subject(s)
Chromatography, High Pressure Liquid/methods , Drugs, Chinese Herbal/analysis , Spectrometry, Mass, Electrospray Ionization/methods , Tablets/analysis , Tandem Mass Spectrometry/methods , Drugs, Chinese Herbal/chemistry , Humans , Tablets/chemistry
12.
J Pharm Biomed Anal ; 170: 68-82, 2019 Jun 05.
Article in English | MEDLINE | ID: mdl-30909056

ABSTRACT

This paper focused on untargeted MSAll, also called MSE, and sequential window acquisition of all theoretical fragment-ion spectra (SWATH) fragmentations for comprehensive structural characterization of triterpene saponins (TSs) in leaves of Acanthopanax senticosus through ultra-high performance liquid chromatography electrospray quadrupole time-of-flight mass spectrometry (UPLC-ESI-QTOF). [M+H]+, [M + NH4]+ and [M + Na]+ precursor ions and the corresponding fragment ions were collected simultaneously in energy-resolved MSAll. SWATH fragmentation was applied as a comparable and complementary method for resolving co-eluting species. A workflow based on MSAll and SWATH fragmentations was constructed for comprehensive structural characterization and rapid discovery of TSs in leaves of A. senticosus. As a result, 89 TSs, along with 14 sapogenins, were unambiguously characterized or tentatively identified. Of these, 33 compounds were characterized as potentially new compounds, including the first report of malonyl-saponin in genus Acanthopanax. This study aimed to systematically analyze TSs in leaves of A. senticosus, and the results are significant for the utilization of A. senticosus leaves.


Subject(s)
Eleutherococcus/chemistry , Plant Leaves/chemistry , Saponins/chemistry , Spectrometry, Mass, Electrospray Ionization/methods , Triterpenes/chemistry , Chromatography, High Pressure Liquid/methods , Plant Extracts/chemistry
13.
Food Chem ; 285: 77-85, 2019 Jul 01.
Article in English | MEDLINE | ID: mdl-30797378

ABSTRACT

Based on QuEChERS dispersed purification, Fe3O4 nanoparticle decoloration and UHPLC-MS/MS, a robust and sensitive method was established for simultaneous analysis of 14 heterocyclic aromatic amines (HAAs) and acrylamide (AA) in coffee products. Sample was extracted by 90% acetonitrile water (v/v), dispersed with primary secondary amine (PSA) and further purified with Fe3O4 nanoparticle. Then, 15 analytes were detected using ESI positive ion under MRM mode. Good linearity was observed for all analytes in the range of 0.2-100 µg/L with the determination coefficients being above 0.996. Limits of detection (S/N ≥ 3) and limits of quantification (S/N ≥ 10) were in the range of 0.02-0.15 µg/L and 0.2-0.7 µg/L, respectively. The intra-day average recoveries were between 81.6% and 100%, and the intra-day precisions ranged from 4.3% to 9.0%. The inter-day average recoveries were in the range of 81.0-101% with precisions ranging from 5.0% to 7.8%. Results indicated that the combination of PSA and Fe3O4 exhibited superior purification and adsorption effects for removing pigments and acid compounds. Real samples analysis indicated that coffee products were widely contaminated with AA, harman and norharman.


Subject(s)
Acrylamide/analysis , Amines/analysis , Ferrosoferric Oxide/chemistry , Metal Nanoparticles/chemistry , Tandem Mass Spectrometry , Acrylamide/standards , Amines/standards , Chromatography, High Pressure Liquid/standards , Coffee/chemistry , Coffee/metabolism , Heterocyclic Compounds/chemistry , Limit of Detection , Reference Standards , Tandem Mass Spectrometry/standards
14.
Nanomicro Lett ; 11(1): 8, 2019 Jan 19.
Article in English | MEDLINE | ID: mdl-34137961

ABSTRACT

Developing an efficient and durable oxygen reduction electrocatalyst is critical for clean-energy technology, such as fuel cells and metal-air batteries. In this study, we developed a facile strategy for the preparation of flexible, porous, and well-dispersed metal-heteroatom-doped carbon nanofibers by direct carbonization of electrospun Zn/Co-ZIFs/PAN nanofibers (Zn/Co-ZIFs/PAN). The obtained Zn/Co and N co-doped porous carbon nanofibers carbonized at 800 °C (Zn/Co-N@PCNFs-800) presented a good flexibility, a continuous porous structure, and a superior oxygen reduction reaction (ORR) catalytic activity to that of commercial 20 wt% Pt/C, in terms of its onset potential (0.98 V vs. RHE), half-wave potential (0.89 V vs. RHE), and limiting current density (- 5.26 mA cm-2). In addition, we tested the suitability and durability of Zn/Co-N@PCNFs-800 as the oxygen cathode for a rechargeable Zn-air battery. The prepared Zn-air batteries exhibited a higher power density (83.5 mW cm-2), a higher specific capacity (640.3 mAh g-1), an excellent reversibility, and a better cycling life than the commercial 20 wt% Pt/C + RuO2 catalysts. This design strategy of flexible porous non-precious metal-doped ORR electrocatalysts obtained from electrospun ZIFs/polymer nanofibers could be extended to fabricate other novel, stable, and easy-to-use multi-functional electrocatalysts for clean-energy technology.

15.
J Pharm Biomed Anal ; 165: 292-303, 2019 Feb 20.
Article in English | MEDLINE | ID: mdl-30576974

ABSTRACT

Optimization of multiple reaction monitoring mass spectrometry (MRM-MS) parameters of triterpene glycosides (TGs) using traditional infusion methods remains to be labor-intensive. However, it was found that mild gas phase decompositions of protonated and ammoninted precursors (DPAP) of TGs could produce a series of abundant dehydrated product ions of aglycones ([A+H-nH2O]+ (n = 0, 1, 2, 3…)) with high efficiency and stability. Based on these considerations and findings, an innovative ESI+-MRM-DPAP-MS strategy was devised on a QTRAP 4000 instrument allowing for rapid the qualitative and quantitative analysis of plant TGs. A detailed study of 85 model compounds from 20 herbal medicines was implemented for validation and evaluation of the ESI+-MRM-DPAP-MS strategy proposed. The central composition design confirmed that collision energy (CE) played more significant roles than declustering potentials (DP) for the formation of these Q1/Q3 ion pairs based on MRM-DPAP-MS. It is also noted that Q1 and Mw were the most important factors for the prediction of CE values by a partial least square regression model. Here, we demonstrated this generic workflow and its merits in: (1) early prediction and selection of MRM ion pairs, no matter which type of TGs, employing a new-found Q1/Q3 calculation formula (Q1=[M+H/NH4]+ and Q3= [A+H-nH2O]+ (n = 0, 1, 2, 3…)); (2) direct determination of practicable CE values using TGs-specific CE-estimating linear equations; (3) appearances of excellent sensitivity, stability and repeatability through real application in Aralia elata, Panax notoginseng and Caulophyllum robustum; (4) seamless application of optimal CE parameters in other triple quadrupole MS instruments such as Thermo TSQ Quantum Ultra. The ESI+-MRM- DPAP-MS may service as an effective and feasible approach for analytical characterization of biological TGs from herbal medicines.


Subject(s)
Glycosides/analysis , Mass Spectrometry/methods , Plant Extracts/chemistry , Triterpenes/analysis , Glycosides/chemistry , Glycosides/isolation & purification , Ions/chemistry , Plants, Medicinal/chemistry , Reproducibility of Results , Triterpenes/chemistry , Triterpenes/isolation & purification
16.
Molecules ; 23(9)2018 Sep 19.
Article in English | MEDLINE | ID: mdl-30235827

ABSTRACT

American ginseng (Panax quinquefolium) has long been cultivated in China for the function food and medicine. Here, ultra-high performance liquid chromatography was coupled with electrospray ionization and triple quadrupole mass spectrometry (UPLC-ESI--TQ-MS) for simultaneous detection of 22 ginsenosides in American ginseng cultivated in Mudanjiang district of Heilongjiang. The extraction conditions also were optimized by a Box Behnken design experiment. The optimized result was 31.8 mL/g as ratio of liquid to raw materials, 20.3 min of extraction time, and 235.0 W of extraction powers. The quantitative MS parameters for these 22 compounds were rapidly optimized by single factor experiments employing UPLC-ESI--multiple reaction monitoring or multiple ion monitoring (MRM/MIM) scans. Furthermore, the established UPLC-ESI--MRM-MS method showed good linear relationships (R² > 0.99), repeatability (RSD < 3.86%), precision (RSD < 2.74%), and recovery (94⁻104%). This method determined 22 bioactive ginsenosides in different parts of the plant (main roots, hairy roots, rhizomes, leaves, and stems) and growth years (one year to four years) of P. quinquefolium. The highest total content of the 22 analytes was in the hairy roots (1.3 × 105 µg/g) followed by rhizomes (7.1 × 104 µg/g), main roots (6.5 × 104 µg/g), leaves (4.2 × 104 µg/g), and stems (2.4 × 104 µg/g). Finally, chemometric methods, hierarchical clustering analysis (HCA) and partial least squares discrimination analysis (PLS-DA), were successfully used to classify and differentiate American ginseng attributed to different growth years. The proposed UPLC-ESI--MRM-MS coupled with HCA and PLS-DA methods was elucidated to be a simple and reliable method for quality evaluation of American ginseng.


Subject(s)
Chromatography, High Pressure Liquid/methods , Ginsenosides/analysis , Panax/chemistry , Spectrometry, Mass, Electrospray Ionization/methods , China , Plant Extracts/chemistry , Plant Leaves/chemistry , Plant Roots/chemistry , Plant Stems/chemistry , Plants, Medicinal/chemistry , Rhizome/chemistry
17.
J Sep Sci ; 41(11): 2354-2359, 2018 Jun.
Article in English | MEDLINE | ID: mdl-29536623

ABSTRACT

A gas chromatography with mass spectrometry method was developed for the simultaneous determination of ten kinds of glycol ethers and their acetates in cosmetics. The samples were extracted with methanol/ethyl acetate (80:20, v/v), further treated with vortex and ultrasound, and analyzed by gas chromatography with mass spectrometry. The concentration of each analyte was calibrated by the external standard method. Under the optimal conditions, the analytes showed linear relationship in the range of 0.05-25 mg/L with determination coefficients larger than 0.9987. The limits of detection and quantification were in the range of 0.09-0.59 and 0.31-1.95 mg/kg, respectively. The average recoveries of three spiked levels were 80.2-105.4% with intra- and interday precisions of 1.1-6.3 and 1.9-6.5%, respectively. Method validation from different labs confirmed the satisfactory recoveries and precisions. This method shows advantages of simple, high sensitivity, and high recovery, which can be applied to the detection of glycol ethers and acetates in cosmetics.


Subject(s)
Acetates/analysis , Cosmetics/analysis , Ethers/analysis , Gas Chromatography-Mass Spectrometry/methods , Glycols/analysis
18.
Food Chem ; 243: 162-167, 2018 Mar 15.
Article in English | MEDLINE | ID: mdl-29146323

ABSTRACT

A sensitive UPLC-MS/MS method was established for the simultaneous determination of seven fluorescent whitening agents in flour matrix. Samples were ultrasonically extracted by trichloromethane-acetone. Then analytes were separated on a C18 column and detected by MS/MS. The developed method was validated in terms of the linearity, matrix effect, accuracy and precision. The method showed a good linearity (r>0.997) for all analytes in their respective concentration ranges. The LOQ for seven analytes were in the range of 2.5-25.0µg/kg. The matrix effect was not significant and almost negligible. The average recoveries of seven analytes from the negative samples spiked at three different concentrations were in a range from 81.5% to 105%. The intra-day precision and inter-day precision were in the ranges of 2.9-9.0% and 6.7-11.2%. The developed method was successfully applied to analyze forty commercial flours and FWA184 was detected in three samples with the concentrations of 31-60µg/kg.


Subject(s)
Bleaching Agents/analysis , Chromatography, High Pressure Liquid/methods , Flour/analysis , Fluorescent Dyes/analysis , Tandem Mass Spectrometry/methods , Bleaching Agents/chemistry , Fluorescent Dyes/chemistry , Reproducibility of Results , Time Factors
19.
J Chromatogr A ; 1526: 31-38, 2017 Dec 01.
Article in English | MEDLINE | ID: mdl-29106962

ABSTRACT

A selective, sensitive and useful method, based on modified QuEChERS cleanup combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the negative-ion electrospray ionization (ESI-) mode, was developed and validated for the simultaneous determination of three inorganic anions including perchlorate (ClO4-), bromate (BrO3-) and hypophosphite (H2PO2-) in flour. The extraction parameters and LC-MS/MS conditions were optimized by single-factor experiment and sorbent combination in modified QuEChERS clean-up was optimized through response surface analysis. Three target analytes were separated on a normal-phase Phenomenex Luna Silica (2) column (150mm×2.0mm, 5µm, 100Å) with the mobile phase of a mixture of 5mmol/L ammonium acetate water solution and acetonitrile, detected by MS/MS under multiple reaction monitoring and quantified by external standard method. The developed method was validated in terms of the sensitivity, linearity, accuracy and precision, and matrix effect. The method showed a good linearity (R2>0.999) for all analytes in their respective concentration ranges. The ILOQs and MLOQs for perchlorate, bromate and hypophosphite were 0.1, 0.5, 5.0µg/L and 2.0, 6.0, 60.0µg/L, respectively. The average recoveries of three target analytes from the negative samples spiked at three different concentrations were in a range from 84.6% to 104.9%. The intra-day precision (n=6) and inter-day precision (n=5) of the target analytes were in the ranges of 2.9%-6.9% and 6.4%-8.2%. The matrix effect of this method was observed between 0.83 and 1.17 and was acceptable. The validated method was successfully applied to determine the concentrations of these inorganic anions in flour. Results found that perchlorate and hypophosphite were detected in 33 out of 50 and 7 out of 50 flour samples.


Subject(s)
Bromates/analysis , Chemistry Techniques, Analytical/methods , Chromatography, Liquid , Flour/analysis , Perchlorates/analysis , Phosphinic Acids/analysis , Tandem Mass Spectrometry , Acetonitriles/chemistry , Chemistry Techniques, Analytical/economics , Chemistry Techniques, Analytical/standards , Limit of Detection , Reproducibility of Results , Solid Phase Extraction
20.
J Mass Spectrom ; 52(12): 848-859, 2017 Dec.
Article in English | MEDLINE | ID: mdl-28929549

ABSTRACT

Forsythia suspensa contains C6 -C2 glucoside conjugates (CCGCs) that are chemically unstable, thereby hindering their isolation and purification. In the present study, ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF) was utilized to screen and identify unstable CCGCs in the fruits and leaves of F. suspensa without any tedious isolation and purified process based on independent information acquisition (also called MSE ) and individual MS/MS experiments. Diagnostic product ion filtering (DPIF) was further applied to mine unknown analogs in MSE high energy levels based on characteristic m/z of key substructures. A modified nomenclature for CCGCs is hereby proposed to facilitate discussions. Possible fragmentation pathways of major types of known CCGCs were proposed and used for deducing their structures. A total of 8 potentially new CCGCs were discovered and initially identified. The accuracy of their identification was further verified by structural elucidation of 3 unstable CCGCs isolated from the fruits of F. suspensa using 1D and 2D-NMR spectroscopy. The established UPLC-QTOF-MSE -based DPIF technique facilitates the rapid discovery and direct identification of unstable CCGCs in fruits and leaves of F. suspensa.


Subject(s)
Chromatography, High Pressure Liquid/methods , Forsythia/chemistry , Glucosides/chemistry , Tandem Mass Spectrometry/methods , Fruit/chemistry , Glucosides/isolation & purification , Ions/chemistry , Magnetic Resonance Spectroscopy/methods , Molecular Structure , Plant Extracts/chemistry , Plant Leaves/chemistry
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