Shimadzu Global COE for Application and Technical Development

Guangzhou, China

Shimadzu Global COE for Application and Technical Development

Guangzhou, China
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Ma Y.,CAS Research Center for Eco Environmental Sciences | Hashi Y.,Shimadzu Global COE for Application and Technical Development | Ji F.,Shimadzu Global COE for Application and Technical Development | Lin J.-M.,Tsinghua University
Journal of Separation Science | Year: 2010

In this study, a simple, rapid and sensitive method for the determination of five phthalates including dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzyl butyl phthalate, and dicyclohexyl phthalate in fruit jellies by LC coupled with MS has been developed. Samples were pretreated by a dispersive SPE method, termed QuEChERS, which is an acronym for quick, easy, cheap, effective, rugged, and safe. The standard calibration curves were linear for all the analytes over the concentration range of 10-250 ng/mL, and the correlation coefficients ranged from 0.9976 to 0.9991. The LODs and LOQs were in the ranges of 0.09-3.68 ng/mL and 0.28-11.25 ng/mL, respectively. The accuracy of this method was evaluated by measuring the recovery from spiked samples. The recoveries of all five phthalates from samples spiked at three different concentrations (0.01, 0.03, and 0.05 mg/kg), were in the ranges of 83.5-103.9%, 86.7-95.8%, and 87.1-95.2%, respectively. The RSD values for the samples spiked at 0.01, 0.03 , and 0.05 mg/kg ranged from 2.0-7.6%, 1.4-6.4%, and 1.2-3.8%, respectively. The method has been used for the analysis of real samples and BBP and DEP were found in real samples. © 2009 Wiley-VCH Verlag GmbH & Co. KGaA.


Lu L.,Beijing University of Chemical Technology | Lu L.,Tsinghua University | Hashi Y.,Shimadzu Global COE for Application and Technical Development | Wang Z.-H.,Beijing University of Chemical Technology | And 2 more authors.
Journal of Pharmaceutical Analysis | Year: 2011

Monolithic silica spin column extraction (MonoSpin-SPE) was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS) to determine the levels of six phthalate esters, dimethyl-(DMP), diethyl-(DEP), dipropyl-[DPrP], butyl-benzyl-(BBP), dicyclohexyl-(DcHP), and di-n-octyl-(DOP) phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges: 0.2-50 μg/L for DMP, DEP, DPrP, DcHP and DOP; 5-100 μg/L for BBP. The correlation coefficients (R 2) were in the range of 0.9951-0.9995 for all the analytes and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02-0.9 μg/L and 0.08-2.7 μg/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs) below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%. DMP and DEP were found in actual physical saline samples (brand A and brand B).


Zhang Q.,Sun Yat Sen University | Zhang Q.,Xingyi Normal University for Nationalities | Li G.,Sun Yat Sen University | Xiao X.,Sun Yat Sen University | And 2 more authors.
Analytical Chemistry | Year: 2016

(Chemical Equation Presented) Cytokinins play a critical role in controlling plant growth and development, but it is difficult to be determined in plant samples due to the extremely low concentration level of picomole/gram. So it is important for efficient sample preparation with selective enrichment and rapid separation for accurate analysis of cytokinins. Herein, a supramolecular perhydroxy-cucurbit[8]uril (PCB[8]) was fabricated into the Fe3O4 magnetic particles via chemical bonding assembly and magnetic perhydroxy-cucurbit[8]uril (MPC) materials were obtained. The MPC had good enrichment capability to cytokinins and the enrichment factors were more than 208. The interaction of MPC and cytokinins was investigated by adsorption test and density functional theory (DFT) calculation, the results showed that the main drive forces were the host-guest interaction and hydrogen-bonding interaction between the perhydroxy-cucurbit[8]uril with analytes. Combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), the MPC was used as a sorbent of magnetic solid-phase extraction for the analysis of cytokinins in plant samples. A sensitive and selective UPLC-MS/MS method was developed with low detection limits of 0.14-0.32 ng/L for cytokinins analysis. Five cytokinins including zeatin riboside, meta-topolin, kinetin, kinetin riboside, and zip with 6.12-87.3 ng/kg were determined in the soybean sprout and Arabidopsis thaliana. The recoveries were in the range of 76.2-110% with relative standard deviations (n = 5) of 2.3-9.7%. On the basis of these results, magnetic perhydroxy-cucurbit[8]uril materials with selective enrichment capability have good potential on the analysis of ultratrace targets from complicated sample matrixes. © 2016 American Chemical Society.


Zhong Q.,Shimadzu Global COE for Application and Technical Development | Qiu X.,Shimadzu Global COE for Application and Technical Development | Lin C.,Shimadzu Global COE for Application and Technical Development | Shen L.,Shimadzu Global COE for Application and Technical Development | And 8 more authors.
Journal of Chromatography A | Year: 2014

An automatic versatile system which integrated solid phase extraction (SPE) with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. Diverse commercial SPE columns can be used under an ambient pressure in this online system realized by a dual-dilution strategy. The first dilution enabled the direct injection of complex samples with minimal pretreatment, and the second dilution realized direct introduction of large volume of strong eluent into the UHPLC column without causing peak broadening or distortion. In addition, a post-column compensation mode was also designed for the matrix-effects evaluation. The features of the online system were systematically investigated, including the dilution effect, the capture of desorption solution, the column-head stacking effect and the system recovery. Compared with the offline UHPLC system, this online system showed significant advantages such as larger injection volume, higher sensitivity, shorter analysis time and better repeatability. The feasibility of the system was demonstrated by the direct analysis of three auxins from different plant tissues, including leaves of Dracaena sanderiana, buds and petals of Bauhinia. Under the optimized conditions, the whole analysis procedure took only 7. min. All the correlation coefficients were greater than 0.9987, the limits of detection and the limits of quantitation were in the range of 0.560-0.800. ng/g and 1.80-2.60. ng/g, respectively. The recoveries of the real samples ranged from 61.0 to 117%. Finally, the post-column compensation mode was applied and no matrix-effects were observed under the analysis conditions. The automatic versatile system was rapid, sensitive and reliable. We expect this system could be extended to other target analytes in complex samples utilizing diverse SPE columns. © 2014 Elsevier B.V.


Leng J.,CAS Shanghai Institute of Organic Chemistry | Zhu D.,Fudan University | Wu D.,Fudan University | Zhu T.,Fudan University | And 2 more authors.
Rapid Communications in Mass Spectrometry | Year: 2012

RATIONALE Peptidomics analysis of human serum is challenging due to the low abundance of serum peptides and interference from the complex matrix. This study analyzed the differentially expressed (DE) low molecular weight peptides in human serum integrating a DMPITC-based N-terminal isotope labeling technique with nano-liquid chromatography and matrix-assisted laser desorption/ionization mass spectrometry (nano-LC/MALDI-MS). METHODS The workflow introduced a [d 6]-4,6-dimethoxypyrimidine-2-isothiocyanate (DMPITC)-labeled mixture of aliquots from test samples as the internal standard. The spiked [d 0]-DMPITC-labeled samples were separated by nano-LC then spotted on the MALDI target. Both quantitative and qualitative studies for serum peptides were achieved based on the isotope-labeled peaks. RESULTS The DMPITC labeling technique combined with nano-LC/MALDI-MS not only minimized the errors in peptide quantitation, but also allowed convenient recognition of the labeled peptides due to the 6 Da mass difference. The data showed that the entire research procedure as well as the subsequent data analysis method were effective, reproducible, and sensitive for the analysis of DE serum peptides. CONCLUSIONS This study successfully established a research model for DE serum peptides using DMPITC-based N-terminal isotope labeling and nano-LC/MALDI-MS. Application of the DMPITC-based N-terminal labeling technique is expected to provide a promising tool for the investigation of peptides in vivo, especially for the analysis of DE peptides under different biological conditions. Copyright © 2012 John Wiley & Sons, Ltd.


Zhong Q.,Shimadzu Global COE for Application and Technical Development | Shen L.,Shimadzu Global COE for Application and Technical Development | Liu J.,Shimadzu Global COE for Application and Technical Development | Yu D.,Shimadzu Global COE for Application and Technical Development | And 8 more authors.
Journal of Chromatography A | Year: 2016

Pre-column dilution large volume injection (PD-LVI), a novel sample injection technique for reverse phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed in this study. The PD-LVI UHPLC-MS/MS system was designed by slightly modifying the commercial UHPLC-MS/MS equipment with a mixer chamber. During the procedure of PD-LVI, sample solution of 200. μL was directly carried by the organic mobile phase to the mixer and diluted with the aqueous mobile phase. After the mixture was introduced to the UHPLC column in a mobile phase of acetonitrile-water (15/85, v/v), the target analytes were stacked on the head of the column until following separation. Using QuEChERS extraction, no additional steps such as solvent evaporation or residue redissolution were needed before injection. The features of PD-LVI UHPLC-MS/MS system were systematically investigated, including the injection volume, the mixer volume, the precondition time and the gradient elution. The efficiency of this approach was demonstrated by direct analysis of 24 pesticides in cabbages. Under the optimized conditions, low limits of detection (0.00074-0.8. ng/kg) were obtained. The recoveries were in the range of 63.3-109% with relative standard deviations less than 8.1%. Compared with common UHPLC-MS/MS technique, PD-LVI UHPLC-MS/MS showed significant advantages such as excellent sensitivity and reliability. The mechanism of PD-LVI was demonstrated to be based on the column-head stacking effect with pre-column dilution. Based on the results, PD-LVI as a simple and effective sample injection technique of reverse phase UHPLC-MS/MS for the analysis of trace analytes in complex samples showed a great promising prospect. © 2016 Elsevier B.V.


Leng J.,CAS Shanghai Institute of Organic Chemistry | Wang H.,CAS Shanghai Institute of Organic Chemistry | Zhang L.,CAS Shanghai Institute of Organic Chemistry | Zhang J.,CAS Shanghai Institute of Organic Chemistry | And 3 more authors.
Journal of the American Society for Mass Spectrometry | Year: 2011

A multifunctional isothiocyanate-based isotope labeling reagent, [d 0]-/[d 6]-4,6-dimethoxy pyrimidine-2-isothiocyanate (DMPITC), has been developed for accurate N-terminus identification in peptide sequencing and comparative protein analysis by ESI Ion-trap TOF mass spectrometry. In contrast with the conventional labeling reagent phenyl isothiocyanate (PITC), DMPITC showed more desirable properties such as rapid labeling, sensitivity enhancement, and facilitating peptide sequencing. More significantly, DMPITC-based labeling strategy possessed the capacity of higher reliable N-terminus identification owning to the high-yield b 1 ion combined with the isotope validation of 6 Da. Meanwhile, it also showed potential in differentiating isomeric residues of leucine and isoleucine at N-terminus on the basis of the relative abundance ratios between the fragment ions of their respective b 1 ions. The strategy not only allows accurate interpretation for peptide but also ensures rapid and sensitive comparative analysis for protein by direct MS analysis. Using trypsindigested bovine serum albumin (BSA), both peptide N-terminus identification and quantitative analysis were accomplished with high accuracy, efficiency, and reproducibility. The application of DMPITC-based labeling strategy is expected to serve as a promising tool for proteome research. © American Society for Mass Spectrometry, 2011.


Li D.-Y.,Xuzhou Medical College | Yan Y.,Xuzhou Medical College | Zhu H.,Xuzhou Medical College | Liu Y.-N.,Xuzhou Medical College | And 6 more authors.
5th International Conference on Bioinformatics and Biomedical Engineering, iCBBE 2011 | Year: 2011

Aims: Hypoxia inducible factor-1α (HIF-1α) plays important roles in response to hypoxia. In this study, the effects of adenovirus mediated transgenic HIF-1α on cardiac function in acute myocardial infarction (AMI) models was investigated. Methods and Results: Ad-HIF-1α (adenovirus vector containing HIF-1α gene) or Rz-HIF-1α group (adenovirus vector containing HIF-1α ribozyme gene) were transfected into myocardial cells respectively. It was discovered that the expression of HIF-1α and VEGF increased at first, reached the peak at 7d (7th day) and decreased gradually from then on. At 56d (56th day), HIF-1α protein was undetectable, and VEGF protein was hardly expressed as well. Meanwhile, the amount of apoptotic cells was the largest in Rz-HIF-1α group, while the one was rather small in Ad-HIF-1α group. Conclusions: In summary, in animal models of myocardial infarction , this adenovirus mediated medical treatment using Ad-HIF-1α gene injection could reverse both the damage to cardiac function and myocardial cell apoptosis under the hypoxia induction. Significance and Impact of the Study: These results may provide an experimental and theoretical proof of adenovirus mediated transgenic HIF-1α in clinical application of myocardial infarction. © 2011 IEEE.

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