Screening for Plant Toxins in Honey and Herbal Beverage by Ultrahigh-Performance Liquid Chromatography-Ion Mobility-Quadrupole Time of Flight Mass Spectrometry

The standards of plant toxins were separated by a C18 column with gradient elution with 0.1% formic acid/water (V/V) and 0.1% formic acid/acetonitrile (V/V) as mobile phase and acquired by ion mobility-quadrupole time of flight mass spectrometry (IM-QTOF MS) in positive ion mode. A database of 308 plant toxins including retention time, collision cross-section (CCS) and its fragment ions was established. Honey dissolved in water or herbal beverage was extracted by acetonitrile and purified with PSA sorbent, and then acquired by ultrahigh-performance liquid chromatography IM-QTOFMS. The acquired data were processed by comparing with the database we established to confirm the target compounds. The average recoveries for samples at two levels ranged from 60.6% - 120.1%, with relative standard deviation (n = 6) less than 25%. The limit of quantitation for plant toxins ranged from 1 - 20 μg/kg. The developed screening method was used in determination of honey, herbal beverage and honey flavored tea beverage samples. The results showed that berberine was detected in one honey with 1 μg/kg and caffeine was present in some beverages with the concentration from 200 and 5500 μg/kg. This method could meet the requirement for rapid screening of plant toxins in honey and herbal beverage. It can be used for the quality control of honey and herbal beverage in enterprises or quality inspection departments. It also can be used in the rapid screening of food poisoning.

Identification of serum biomarkers for diagnosing stage Ⅰ lung adenocarcinoma by MALDI-TOF mass spectrometry

Objective To identify specific biomarkers that could improve early diagnosis of lung adenocarcinoma using matrix-assisted laser desorption/ionization (MALDI) technology. Methods Serum samples were isolated from 17 patients with stage Ⅰ lung adenocarcinoma and 17 age-and sex-matched healthy controls,and the serum proteomic profiles were obtained by matrix-assisted laser desorption ionization time of flight (MALDI-TOF) mass spectrometry. Results Compared with healthy control group,two highly expressed potential biomarkers were identified with the relative molecular weights of 6 631.64 Da and 4 964.21 Da. The two best novel protein peaks were automatically chosen for the system training and the development of the constructed model. The constructed model was then used to test an independent set of masked serum samples from 15 lung adenocarcinoma patients and 22 healthy individuals. The analysis yielded a sensitivity of 93.3%,and a specificity of 95.5%. Conclusion These results suggest that MALDI-TOF-MS ProteinChip technology is a quick,convenient,and high-output analyzing method that is capable of selecting several relatively potential biomarkers from the serum of lung adenocarcinoma patients and may have a clinical value in the future,and will provide clues to identifying new serologic biomarkers of lung adenocarcinoma.

Establishment and Preliminary Application of Two dimensional Electrophoresis and Mass Spectrometry in Ovary Study

Objective To apply two-dimensional electrophoresis and mass spectrometry in the ovary proteome researchMethods Protein extractions from mouse ovaries were run in IPGphor isoelectric focus system with 11 cm and 24 cm IPG strips respectively (pH 3～10, 0.3 mm thick), then the protein spots were identified by mass spectrometry.Results The ovary protein exactions separated by two-dimensional electrophoresis have got high resolution, and identifing protein by mass spectrometry was highly efficient and facilitly. These two techniques should facilitate further investigation of female reproduction proteome research.Conclusion These two rapid high resolutions and efficient techniques have a variety of applications foreground in female reproduction proteome pattern research.

Exact Mass Measurements for α-Allenic Alcohol by Atmospheric Pressure Chemical Ionization/Time-of-flight Mass Spectrometry

The atmospheric pressure chemical ionization/time of flight mass spectrometry (APCI/TOF MS) was applied to determine the mass of five α allenic alcohols via their protonated molecular ions using positive ion mode. Polyethylene glycol (PEG) was used as the internal reference. All results were obtained under the resolution of about 5000 FWHM (full width at the half maximum). Solvent effects were studied and the satisfied results were obtained in acetonitrile. Compared with the theoretical values, all absolute errors were less than 1.0 mmu. The effects of nozzle potential, push pulse potential, pull pulse potential, pull bias potential and acquisition rate on exact mass determination were also discussed. APCI/TOF MS is proven to be a very sensitive analytical technique and an alternative ionization mode in analyzing thermally labile compounds with relatively weak polarity, such as α allenic alcohol.

Diagnosis of Tumor-Like Polypoid Lesions of Gallbladder by Serum Proteomic Fingerprint

Objective： To search the specific serum proteins in tumor-like polypoid lesions of the gallbladder（PLG） patients. Methods： Surface enhanced laser desorption/ionization time of flight mass spectrometry （SELDI-TOF-MS） technique and WCX Magnetic Beads were used to detect the serum proteomic fingerprint of 23 patients with tumor-like PLG, 21 patients with non tumor-like PLG and 26 normal persons. Biomarker Wizard and Biomarker Patterns Software were used in combination to analyze the data. Results： In the preliminary screening, 22 representative specific proteins for tumor-like PLG were found. Seven specific proteins showed increased expression and 15 specific proteins showed decreased expression in the tumor-like PLG patients. Three specific proteins are selected for the diagnosis of the tumor-like PLG.. Conclusion： SELDI-TOF-MS technique can be used to select specific proteins for tumor-like PLG patients, which may be useful for the diagnosis of the tumor-like PLG and the differential diagnosis with the non tumor-like PLG.

A depressant for marmatite flotation:Synthesis,characterisation and floatation performance

This study synthesised a zincic salt(ZS)as a depressant for marmatite-galena separation.The effect of ZS on the flotation of marmatite and galena was investigated through micro-flotation tests.88.89%of the galena was recovered and 83.39%of the marmatite was depressed with ZS dosage of 750 mg·L^(−1)at pH=4.The depression mechanism of ZS on marmatite was investigated by a variety of techniques,including adsorption measurements,Fourier transform infrared(FTIR),X-ray photoelectron spectroscopic(XPS)analysis,and time of flight secondary ion mass spectrometry(ToF-SIMS).Results of adsorption tests and FTIR reveal that ZS adsorbed on marmatite surface and impeded the subsequent adsorption of butyl xanthate(BX).The results of XPS and ToF-SIMS indicate that the ZnO_(2)^(3-)released by ZS could be chemisorbed on the marmatite surface and depress marmatite flotation.

Low-resistance ohmic contacts on InAlN/GaN heterostructures with MOCVD-regrown n+-InGaN and mask-free regrowth process

This paper studied the low-resistance ohmic contacts on InAlN/GaN with metal–organic chemical vapor deposition(MOCVD)regrowth technique.The 150-nm regrown n-InGaN exhibits a low sheet resistance of 31Ω/□,resulting in an extremely low contact resistance of 0.102Ω·mm between n^(+)-InGaN and InAlN/GaN channels.Mask-free regrowth process was also used to significantly improve the sheet resistance of InAlN/GaN with MOCVD regrown ohmic contacts.Then,the diffusion mechanism between n^(+)-InGaN and InAlN during regrowth process was investigated with electrical and structural characterizations,which could benefit the further process optimization.

新型减肥药利莫纳班的离子阱质谱和电子轰击质谱研究

Rimonabant was studied by ESI ion trap mass spectrometry and EI(electron impact) time-of-flight mass spectrometry.m/z 380.9 can be used for identification of this drug by LC-MS.An exact mass at m/z 462.0782 (calculated 462.0781) with abundance (8.56%) in the spectra was found for its molecular ion.Ten characteristic fragment peaks with relatively strong intensities were observed,which can be used for identification of this drug.

LCT和GCT联合鉴别未知水样中N,N-二烷基氨基乙基磺酸及其类似物

N,N-dialkylaminoethane-2-sulfonic acids are environmental marker compounds of V type nerve agents,hence analysis of them is very important for verification of the chemical weapons convention(CWC).In this article,liquid chromatography-high resolution time of flight mass spectrometry coupled with accurate mass measurement were used to discriminate N,N-disopropyl aminoethane-2-sulfonic acid and a CWC non-related compound 3-(N-Morpholino)propanesulfonic acid in Water.The method was fast,simple and accurate,proving that high resolution mass spectrometry is a good technique for the analysis of unknown toxicant.

Direct thrust test and asymmetric performance of porous ionic liquid electrospray thruster

In order to meet the demand of CubeSats for low power and high-performance micro-propulsion system,a porous ionic liquid electrospray thruster prototype is developed in this study.1010 conical emitter arrays are fabricated on an area of 3.24 cm^(2) by computer numerical control machining technology.The propellant is 1-ethyl-3-methylimidazolium tetrafluoroborate.The over-all dimension of the assembled prototype is 3 cm×3 cm×1 cm,with a total weight of about 15 g(with propellant).The performance of this prototype is tested under vacuum.The results show that it can work in the voltage range of±2.0 kV to±3.0 kV,and the maximum emission current and input power are about 355 lA and 1.12 W.Time of Flight(TOF)mass spectrometry results show that cationic monomers and dimers dominate the beam in positive mode,while a higher proportion of higher-order solvated ion clusters in negative mode.The maximum specific impulse is 2992 s in positive mode and 849 s in negative mode.The thrust is measured in two methods:one is calculated by TOF results and the other is directly measured by high-precision torsional thrust stand.The thrust(T)obtained by these two methods conforms to a certain scaling law with respect to the emis-sion current(I_(em))and the applied voltage(V_(app)),following the scale of T-Iem_(Vapp)^(0.5),and the thrust range is from 2.1 lN to 42.6 lN.Many thruster performance parameters are significantly different in positive and negative modes.We speculate that due to the higher solvation energy of the anion,more solvated ion clusters are formed rather than pure ions under the same electric field.It may help to improve thruster performance if porous materials with smaller pore sizes are used as reservoirs.Although there are still many problems,most of the performance parameters of ILET-3 are good,which can theoretically meet the requirements of CubeSats for micro-propulsion system.

Reactions of Laser Ablated Metal Plasma with Molecular Alcohol Beams： Dependence of the Produced Cluster lon Species on the Beam Condition

The gas phase reactions of metal plasma with alcohol clusters were studied by time of flight mass spectrometry （TOFMS） using laser ablation-molecular beam （LAMB） method. The significant dependence of the product cluster ions on the molecular beam conditions was observed. When the plasma acted on the low density parts of the pulsed molecular beam, the metal-alcohol complexes M^＋An （M=Cu, Al, Mg, Ni and A=C2H5OH, CH3OH） were the dominant products, and the sizes of product ion clusters were smaller. While the plasma acted on the high density part of the beam, however, the main products turned to be protonated alcohol clusters H^＋An and, as the reactions of plasma with methanol were concerned, the protonated water-methanol complexes H3O^＋（CH3OH）n with a larger size （n≤12 for ethanol and n≤24 for methanol）. Similarly, as the pressure of the carrier helium gas was varied from 1 × 10^5 to 5 × 10^5 Pa, the main products were changed from M^＋An to H^＋An and the sizes of the clusters also increased. The changes in the product clusters were attributed to the different formation mechanism of the output ions, that is, the M^＋An ions came from the reaction of metal ion with alcohol clusters, while H^＋An mainly from collisional reaction of electron with alcohol clusters.

Inhibition of galvanic corrosion in Al/Cu coupling model by synergistic combination of 3-Amino-1,2,4-triazole-5-thiol and cerium chloride

Asynergistic inhibition study was carried out on an aluminium/copper galvanic coupling model in neutral aerated NaCl solution using scanning vibrating electrode technique(SVET).The approach allows the simulation of the local micro-galvanic cells of AA2024-T3 obtained from the potential difference between the intermetallic particles(IMPs)and the aluminium matrix.The inhibition effect of CeCl3 and 3-Amino-1,2,4-triazole-5-thiol(ATAT)was demonstrated by the reduction in the galvanic current density over Al and Cu surfaces.An improved inhibition from positive synergistic effect was revealed by the combination of the two inhibitors after 24 h of immersion,with the best inhibition recorded for Ce1.5ATAT3.5.Scanning electron microscopy(SEM),X-ray photoelectron spectroscopy(XPS)and time of flight secondary ion mass spectrometry(ToF-SIMS)were used to characterize the Ce-and ATAT-based complex film formed and to illustrate the mechanism of inhibition.

Proteomics analysis of cerebral cortex in Wistar rats

To analyze the protein expression pattern of the cerebral cortex in Wistar rats using the proteomics approach,proteins were separated by two-dimensional gel electrophoresis,stained with Coomassie brilliant blue and digested with trypsin.Then,we analyzed the peptide section using a matrix-assisted laser desorption/ionization time of flight mass spectrometry(MALDI-TOF-MS)and identified the protein by indexing special database(SwissProt)according to the finger printing of the peptide quality.Eighty-four protein spots were identified,including metabolic enzymes,skeleton proteins,heat shock proteins,antioxidant proteins,signaling proteins,proteasome related proteins,neuron and glial specific proteins and serum associated proteins.The result of this study enriches the database of the proteome in the cerebral cortex of rats and lays a foundation for further research of neurological disorders in rat models.

α2,3-Sialylation with Fucosylation Associated with More Severe Anti-MDA5 Positive Dermatomyositis Induced by Rapidly Progressive Interstitial Lung Disease

Dermatomyositis(DM)is a heterogeneous autoimmune disease associated with numerous myositis specific antibodies(MSAs)in which DM with anti-melanoma differentiation-associated gene 5-positive(MDA5+DM)is a unique subtype of DM with higher risk of developing varying degrees of Interstitial lung disease(ILD).Glycosylation is a complex posttranslational modification of proteins associated with many autoimmune diseases.However,the association of total plasma N-glycome(TPNG)and DM,especially MDA5+DM,is still unknown.TPNG of 94 DM patients and 168 controls were analyzed by mass spectrometry with in-house reliable quantitative method called Bionic Glycome method.Logistic regression with age and sex adjusted was used to reveal the aberrant glycosylation of DM and the association of TPNG and MDA5+DM with or without rapidly progressive ILD(RPILD).The elastic net model was used to evaluate performance of glycans in distinguishing RPLID from non-RPILD,and survival analysis was analyzed with N-glycoslyation score by Kaplan-Meier survival analysis.It was found that the plasma protein N-glycome in DM showed higher fucosylation and bisection,lower sialylation(α2,3-notα2,6-linked)and galactosylation than controls.In MDA5+DM,more severe disease condition was associated with decreased sialylation(specificallyα2,3-sialylation with fucosylation)while accompanying elevated H6N5S3 and H5N4FSx,decreased galactosylation and increased fucosylation and the complexity of N-glycans.Moreover,glycosylation traits have better discrimination ability to distinguish RPILD from non-RPILD with AUC 0.922 than clinical features and is MDA5-independent.Survival advantage accrued to MDA5+DM with lower N-glycosylation score(p=3e-04).Our study reveals the aberrant glycosylation of DM for the first time and indicated that glycosylation is associated with disease severity caused by ILD in MDA5+DM,which might be considered as the potential biomarker for early diagnosis of RPILD and survival evaluation of MDA5+DM.