[Application progress of on-line sample preparation techniques coupled with liquid chromatography-mass spectrometry system in the detection of food hazards].

Food safety has received increased attention, and food detection is of great significance. The food matrix is complex, and diverse food hazards have been identified. Thus, the detection methods and sample preparation techniques for food matrices must be continuously optimized and updated. Several steps are usually required when a chromatographic system is used to determine food hazards: sample preparation, that is, the separation of targets from different substrates using a suitable preprocessing method and target-substance separation and purification, which is usually achieved using chromatographic separation. The selection of an appropriate detector for qualitative and quantitative analyses is usually based on the properties of the target compound. The sample preparation procedure is considered the most time-consuming aspect of the entire food-analysis process. It is also prone to analytical errors. Therefore, optimization of the sample preparation process is a key issue in the field of chemical analysis. Researchers have developed a series of new, efficient, and accurate sample preprocessing methods, and an on-line sample-preparation system has been found to be a feasible approach. On-line sample preparation coupled with liquid chromatography-mass spectrometry (LC-MS) presents many advantages. First, manual operation could reduce analytical errors to ensure good accuracy and repeatability. It could also reduce the consumption of chemical reagents and avoid cross-contamination between samples. Furthermore, an on-line sample-preparation system could shorten the sample-preparation time and improve the detection efficiency. On-line sample preparation coupled with LC-MS has been widely applied in the fields of environment, biology, and food. On-line sample preparation systems coupled with LC-MS are divided into two modules: the first modules involves sample preparation and the second module involves the LC system. The first module remove impurities and isolates the target compounds in preparation for their qualitative and quantitative detection. The coupling of these two modules depends mainly on valve switching. In this paper, we introduce the most frequently used on-line sample-preparation techniques, including on-line solid phase extraction (on-line SPE), in-tube solid phase microextraction (in-tube SPME), and turbulent chromatography (TFC). We then describe the basic principles and coupling equipment of these three on-line analytical technologies in detail. The coupling equipment establishes a physical connection between the two modules. Next, we discuss the properties of different purification fillers in an on-line sample-preparation column. The applications and research progress of on-line systems for pesticide residues, veterinary drug residues, and biotoxins are also discussed. Compared with offline sample preparation, on-line analytical systems present several advantages. On-line analytical systems can not only greatly reduce the analysis time and solvent consumption but also improve the detection sensitivity and accuracy. Such systems can be used to determine food hazards to ensure food safety. Finally, the existing problems and development trends of on-line analytical systems are discussed and prospected. To promote the applications of on-line analytical technology in food-safety detection, we suggest that the following three aspects be considered. First, more on-line purification columns with novel fillers, in addition to C18 or polymer fillers, should be developed. Second, compared with ordinary detectors, high-resolution MS detectors have better precision and accuracy. Coupling on-line analytical technologies with a high-resolution mass spectrometer may be beneficial for the further development of on-line analyses. Third, different food matrices should be compared and evaluated to continuously optimize the detection process and improve the efficiency of on-line analytical systems. As concerns regarding food safety issues have increased, the applications of on-line analytical technologies for food detection can be expected to become increasingly important.

Fine nursing model combined with psychological intervention on patients after eyeball enucleation due to ocular trauma.

PURPOSE: To study the effect of fine nursing model combined with psychological intervention on quality of life and psychological state of patients after eyeball enucleation due to ocular trauma. METHODS: 80 patients with eyeball enucleation due to ocular trauma admitted to our hospital from January 2017 to July 2019 were randomly selected and divided into control group and experimental group by coin tossing, with 40 patients in each group. Patients in the control group received routine nursing care, and patients in the experimental group received refined nursing with psychological intervention. Quality of life index (QLI) score, pittsburgh sleep quality index (PSQI) quality of sleep score, mental state assessment scale (MSSNS) score, self-rating anxiety scale (SAS), self-rating depression scale (SDS) score, nursing efficiency, nursing satisfaction were compared between the two groups. RESULTS: The experimental group showed a statistically significant increase in the QLI quality of life scores as compared with the control group (P < 0.05); The PSQI quality of sleep score, MSSNS psychological status score, SAS, SDS anxiety, depression scale scores were found to be markedly lower in the experimental group than those observed in the control group, and the difference was proven to be statistically significant (P < 0.05); The nursing satisfaction and nursing efficiency were reported at a notably higher rate in the experimental group compared to what were observed in the control group, and the difference indicated a statistical significance (P < 0.05). CONCLUSION: Fine nursing combined with psychological intervention could significantly improve quality of life of patients, improve their psychological state and sleep quality, and help to raise nursing satisfaction and nursing efficiency. Therefore, fine nursing combined with psychological intervention has a higher application value in patients with traumatic eyeball extraction.

A stable and sensitive enzyme-linked immunosorbent assay (ELISA) for the determination of metsulfuron-methyl residues in foods.

A hapten of metsulfuron-methyl was successfully designed and synthesized from 2-methylester-phenylsulfonamide and succinic anhydride, and the polyclonal antibody against metsulfuron-methyl was prepared by immunization procedure with the hapten-bovine serum albumin conjugate. A stable and sensitive direct competitive enzyme-linked immunosorbent assay (dcELISA) method had been developed under the optimal conditions. The sensitivity (IC50 ) was 37.03 ± 1.87 µg/L, and the detection line (IC15 ) was 1.57 ± 0.11 µg/L. Rice, wheat, oat, flaxseed, milk, and water were chosen to study the recovery test and the recovery rates were 83.11%-117.44% . The matrix effect was eliminated by a simple dilution of the sample extracts. The results from dcELISA were well agreement with the results from HPLC-MS. It was indicated that the developed method had good accuracy and stability. It could be applied for the detection of metsulfuron-methyl residues. It was worth mentioning that the antibody could recognize metsulfuron-methyl and tribenuron-methyl with cross-reactivities of 100% and 49.72%, respectively. In order to understand the cross-reactivity, molecular modeling including molecular alignment and electrostatic potential surfaces were introduced. It was found that the special group of metsulfuron-methyl played an important role, especially on C3 position of the phenyl group. PRACTICAL APPLICATION: A stable, sensitive, and low-cost dc ELISA method had been developed with good accuracy and applied in the determination of metsulfuron-methyl in foods. Molecular simulation was introduced to understand the specificity between the antibody and the analyst. It was a good method to study the cross-reactivity between the antibody and the analyst or analogue.

Determination of Deoxynivalenol and Its Derivative in Corn Flour and Wheat Flour Using Automated On-line Solid-Phase Extraction Combined with LC-MS/MS.

An automated on-line solid-phase extraction (SPE) combined with LC-MS/MS method was developed for determination of deoxynivalenol (DON), 3-acetyl-DON and 15-acetyl-DON in corn flour and wheat flour samples. The extraction solvent of the samples was injected into the automated on-line SPE system to remove matrix interference. After washing step, the targets were eluted from the SPE cartridge into liquid chromatography (LC) column. Several SPE parameters including injection volume, elution volume and eluting flow rate were assessed and optimized. Method validation was evaluated and good linearity was obtained (R2 > 99%) with the limit of detection of 0.1-0.2 µg/kg. Recoveries were evaluated in spiked corn flour and wheat flour samples at three concentrations and the values ranged from 86.5% to 99.7%. The benefit of the present method with automated on-line SPE system is the ability to inject directly pure extracts into LC-MS/MS, offering faster analyses and improving analysis efficiency.

Novel magnetic fluorescence probe based on carbon quantum dots-doped molecularly imprinted polymer for AHLs signaling molecules sensing in fish juice and milk.

A magnetic fluorescence probe was fabricated by coating carbon quantum dots-doped molecularly imprinted polymers (MIPs) layers on the surface of Fe3O4 particles (MFMP) for detection of N-acyl homoserine lactones (AHLs) signaling molecules. N-Z-L-homoserine lactone molecular was used as the template to prepare AHLs MIP layers, employing MAA and HEMA as functional monomers. The developed MFMP owned superparamagnetism, fluorescence, fast response and class-selectivity. If AHLs (C4-HSL, C6-HSL, C8-HSL, C10-HSL, C12-HSL and C14-HSL) were captured by the MFMP, they quenched the fluorescence of the probe. Fluorescence dropped linearly in the concentration ranges of 3.65 × 10-3 µmol/L-0.96 × 10-1 µmol/L for AHLs. The MFMP was applied to the analysis of fish juice and milk samples, and recoveries ranged from 83.10% to 90.74% with relative standard deviation less than 5.1%. This study offered a novel strategy to fabricated AHLs fluorescence probe with great potential for wide-ranging application in agri-food products.

[Determination of ten alkaloids in cosmetics by high performance liquid chromatography-tandem mass spectrometry].

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of ten alkaloids in cosmetics. Extraction conditions, purification methods and instrumental parameters were optimized. The samples were ultrasonically extracted with 80% (v/v) methanol aqueous solution. The extracts were separated and filtered after centrifugation. The analytes were separated on a Waters BEH C18 column, and detected in the selected reaction monitoring mode. Ten alkaloids were quantified by the external standard method. The ten alkaloids showed good linearity with correlation coefficients (R2) greater than 0.9900. The limits of detection (LODs) and the limits of quantification (LOQs) of the ten alkaloids were in range of 5.0-12.5 µg/kg and 12.5-50.0 µg/kg, respectively. The average spiked recoveries in the cosmetics ranged from 70.91% to 116.75%, and the relative standard deviations (RSDs) ranged from 0.49% to 9.98%. The method can be used for the rapid screening and quantitative analysis of ten alkaloids in cosmetics.

A novel approach for fluorescent visualization of glycyrrhetic acid on a cell with a quantum dot.

Glycyrrhetic acid (GA), a pentacyclic triterpenoid derivative obtained from hydrolysis of glycyrrhizic acid, was found to have synergistic anti-asthmatic effects with the ß2-adrenergic receptor (ß2AR) agonist via the ß2AR-mediated pathway. This study visualized the location of GA on a human cell expressing ß2AR via chemical biological approaches. A CdTe/ZnS quantum dot modified with an alkynyl group (QD-AL) was first synthesized, and an azide-terminal GA (ATGA) was also prepared. The QD-AL was used for fluorescence visualization of the distribution of GA on human embryonic kidney 293 cells expressing fusion ß2AR (HEK293-ß2AR) through the "click reaction" between QD-AL and ATGA. The average size of the QD-AL nanoparticle was about 10 nm, and its fluorescent emission wavelength was 620 nm. The location of GA on the HEK293-ß2AR cell membrane can be visualized by the click reaction (between QD-AL and ATGA). The ability of QD-AL targeting to ATGA on the cell membrane of a HEK293-ß2AR cell was further investigated using both confocal laser-scanning microscopy and a cellular uptake-inhibition assay. The results reveal that QD-AL can recognize ATGA on the cell membrane through the click reaction, which provides a new approach for visualizing the location of GA on the cell in an indirect way, and it can be applied to explore the synergistic anti-asthmatic mechanism of GA with ß2AR agonist through the ß2AR mediated pathway.

Schiff base-chitosan grafted multiwalled carbon nanotubes as a novel solid-phase extraction adsorbent for determination of heavy metal by ICP-MS.

A novel Schiff base-chitosan-grafted multiwalled carbon nanotubes (S-CS-MWCNTs) solid-phase extraction adsorbent was synthesized by covalently grafting a Schiff base-chitosan (S-CS) onto the surfaces of oxidized MWCNTs. The adsorbent was characterized by Fourier-transform infrared spectroscopy, transmission electron microscopy, and thermal gravimetric analysis. The results showed that S-CS was successfully grafted onto the surfaces of MWCNTs. A method was developed for the determination of heavy metals, namely V(V), Cr(VI), Cu(II), As(V) and Pb(II) in biological and environmental samples by inductively coupled plasma mass spectrometry coupled with preconcentration with S-CS-MWCNTs. The parameters influencing preconcentration of target ions, such as the pH of the sample solution, the flow rate of sample loading, the eluent concentration, and eluent volume, were investigated and optimized. Under the optimal conditions, the enrichment factors of V(V), Cr(VI), Cu(II), As(V), and Pb(II) reached 111, 95, 60, 52, and 128, respectively, and the detection limits were as low as 1.3-3.8 ng L(-1). The developed method was successfully applied to the determination of trace-metal ions in herring, spinach, river water, and tap water with good recoveries ranging from 91.0% to 105.0%.

Cell surface glycoprotein profiling of cancer cells based on bioorthogonal chemistry.

Bioorthogonal chemistry refers to chemical reactions that can occur within a living system without altering native biochemical processes. Applications of this concept extend to studies on a group of biomolecules that includes glycans, proteins, and lipids. In this study, a strategy for isolating cell surface glycoproteins and based on bioorthogonal chemistry was employed to identify new cancer-related glycoproteins. A novel alkyne reagent containing one disulfide bond was synthesized for the enrichment of glycoproteins metabolized with peracetylated N-azidoacetylmannosamine, which was applied on three different cancer cell lines, and all isolated proteins were analyzed by high-performance liquid chromatography-tandem mass spectrometry. The strategy of purifying cell surface glycoproteins introduced in this article was shown to be reliable, and a total of 56 cell surface glycoproteins were identified. Neuronal cell adhesion molecule was found uniquely expressed in A549 lung adenocarcinoma, and its expression in non-small-cell lung carcinomas was detected by immunohistochemistry. Furthermore, a significant increase of neuronal cell adhesion molecule expression was identified in non-small-cell lung adenocarcinoma compared with adjacent noncancerous tissues, and could be a novel potential target and marker in cancer treatment and detection.

Synthesis of novel folate conjugated fluorescent nanoparticles for tumor imaging.

A novel folate fluorescent nanoconjugate was synthesized and used for detection of cancer cells overexpressing the folate receptor (FR). The folate conjugate (PCMS-NA-FA) was synthesized by conjugating folic acid (FA) and 4-ethylnyl-N-ethyl-1, 8-naphthalimide (NA) to the polychloromethylstyrene (PCMS) functionalized with azido group (PCMS-N3) through click reaction. The obtained conjugate had clear structure and could form PCMS-NA-FA nanoparticles with particle size around 86 nm in aqueous solution. Ability of PCMS-NA-FA targeting to cancerous cells was investigated by comparing the uptake of the nanoparticles by human adenocarcinoma HeLa cells and by non-FR expressing human lung carcinoma A549 cells. Specificity of the PCMS-NA-FA nanoparticles targeting on FRs was verified with cellular uptake inhibition assay, in which HeLa cells were incubated with both nanoconjugate and free FA. In addition, the specificity was also confirmed by the collocation of the immunofluorescence staining of anti-FR and the cellular uptake of the PCMS-NA-FA nanoparticles. Furthermore, the organ distribution of this folate nanoconjugate was studied on HeLa cell-bearing mice via frozen slicing, and the results showed that the folate nanoparticles were preferentially accumulated in the tumor site rather than other tissues, indicating the desired specificity for tumor targeting and imaging. All these findings suggested that this practical synthetic strategy can potentially facilitate the preparation of multifunctional imaging probe in biology and diagnosis of disease.