High Performance Liquid Chromatography-mass Spectrum Research Articles

Effects of phenolic acid grafted-chitosan hydrocolloids on the aldehyde contents from lipid oxidation in golden pompano (Trachinotus blochii) fillets during pan-frying

The effects of phenolic acid grafted-chitosan hydrocolloids (CS-g-GA/FA) on aldehyde contents from lipid oxidation in golden pompano fillets during pan-frying was investigated with an established high-performance liquid chromatography-mass spectrum method. Results indicated that pan-frying induced profound lipid oxidation and aldehydes generation with propanal, hexanal, nonanal, trans, trans-2,4-decadienal, and 4-hydroxy-2-nonenal as the abundant species. CS-g-FA and CS-g-GA effectively decreased their contents by 23.74–27.42 %, 61.69–67.42 %, 41.83–53.91 %, 29.91–48.79 %, and 61.57–65.39 % after 3 min. Most aldehyde contents decreased with the extension of pan-frying time due to the volatilization and reaction. In terms of substrate depletion, CS-g-phenolic acids effectively inhibited unsaturated fatty acids oxidation due to their decent antioxidant activity than CS. The significant lower retention rates of aldehydes in the CS-g-phenolic acids groups compared with control in chemical mode confirmed the carbonyl ammonia condensation. These results suggested that CS-g-phenolic acids serve as novel coating to reduce hazardous compounds during aquatic products thermal processing.

Synthesis, characterization and evaluation of a pH-responsive molecular imprinted polymer for Matrine as an intelligent drug delivery system

Abstract To address the undesirable reactions associated with matrine (MAT) injection in clinical settings, a high-loading drug delivery system (DDS) based on pH-sensitive molecularly imprinted polymer (MAT@MIPs) was prepared for the first time. The imprinted materials containing recognition sites for the matrine were formed by using carboxyl-functionalized multiwalled carbon nanotubes as a supportive matrix and dopamine as a cross-linker due to its exceptional biocompatibility. Subsequently, the optimal reaction conditions and adsorption performance of MAT@MIPs were systematically investigated. The obtained polymers were characterized and evaluated by Fourier transform infrared spectrometry, scanning electron microscopy, elemental analysis, and thermogravimetric analysis. Results indicated that the MIPs demonstrated a favorable imprinting factor (2.36) and a high binding capacity (21.48 mg·g−1) for matrine. In vitro studies, we performed cell counting kit-8 assays in HepG2 cells, then the drug delivery capabilities of MAT-loaded MIPs were validated through light microscopy analyses, and the matrine content in culture medium was quantified using ultra high-performance liquid chromatography-mass spectrum synchronously. The facile fabrication of MAT@MIPs presents a viable solution for designing high-loading and pH-responsive DDS, which can offer a novel administration approach for drugs requiring injection in clinical applications.

Screening and characterizing the quality markers of Selaginella tamariscina (P. Beauv.) Spring using metabonomics and molecular networking

Quality control of traditional Chinese medicine (TCM) should be linked with the authentication and efficacy of TCM. Selaginella tamariscina is a frequently used traditional Chinese herbal medicine. However, its quality control is still difficult due to its multiple adulterants. We established quality markers (Q-markers) of S. tamariscina by using metabolomics, molecular networking and network pharmacology to improve the authenticity study and quality control of S. tamariscina. In this study, ultra high performance liquid chromatography-mass spectrum (UHPLC-MS) coupled with multivariate statistical analyses was applied to distinguish between S. tamariscina samples and their confusing adulterants. Principal component analysis, hierarchical clustering analysis (PCA), hierarchical clustering analysis (HCA) and partial least squares discriminant analysis (PLS-DA) were employed to screen the distinguishing markers from S. tamariscina samples and their adulterants. The top-2 distinguishing markers were isolated from S. tamariscina and identified by molecular networking together with nuclear magnetic resonance spectroscopy (NMR). Network pharmacology predicted the bioactivity and cytotoxicity of the top-2 distinguishing markers. The top-2 distinguishing markers were adopted as Q-markers of S. tamariscina for content determination. Based on the results of ultra performance liquid chromatography-quardrupole-time of flight mass spectrometry (UHPLC-QTOF-MS) metabolomics, we revealed that selaginellins could only be detected in S. tamariscina samples and contributed greatly to discriminating S. tamariscina samples from their confused species. The top-2 distinguishing markers were isolated and purified from S. tamariscina extract. Then, they were further identified as selaginellin and selaginellin A by molecular networking and NMR. Network pharmacology predicted the antitumor activity of selaginellin and selaginellin A, while the cytotoxicity assay verified their bioactivity. In conclusion, selaginellin and selaginellin A were selected as Q-markers for the determination and quality evaluation of S. tamariscina based on ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UHPLC-QQQ-MS). The ranges of the concentrations of selaginellin and selaginellin A were 41.57–44.89 μg/g and 15.09–16.75 μg/g, respectively. This study provides a novel strategy combining Ultra performance liquid chromatography mass spectrometry based (UHPLC-MS-based) metabolomics with molecular networking for rapid species identification of S. tamariscina and discovery of the Q-markers of TCM.

Determination of sulfonamides in meat by monolithic covalent organic frameworks based solid phase extraction coupled with high-performance liquid chromatography-mass spectrometric

In this work, hierarchical porous covalent organic frameworks (HP-COFs) foam, named as HP-TpBD, was prepared by using 1,3,5-trimethylphloroglucinol (Tp) and benzidine (BD) as building blocks under the assistant of NaCl template. Its potential application as the sorbent for solid phase extraction (SPE) of sulfonamides (SAs) in meat products were explored by coupling with high performance liquid chromatography-mass spectrum (HPLC-MS) analysis. The key factors affecting extraction efficiency were well studied. Under the optimum conditions, the proposed method exhibited high preconcentration factors of 100, low limit of detection (0.10-0.23 μg/kg), and wide linear ranges (0.5-200 μg/kg). In addition, the determination of SAs in real samples were realized with satisfactory recoveries (82.8-119.9%), demonstrating the applicability of the proposed method. The easy operation, superior extraction affinity and good recycle performance demonstrated the resulting HP-COF foam is a promising adsorbent for the preconcentration of trace organic compounds from complex matrix.

Singlet oxygen mediated the selective removal of oxytetracycline in C/Fe3C/Fe0 system as compared to chloramphenicol

Reactive oxygen species (ROS) production for Fe0 is limited because of the formed iron corrosion products. In this study, C/Fe3C/Fe0 composite which produces enhanced ROS has been specifically designed and fabricated to remove typical antibiotics (i.e., oxytetracycline (OTC) and chloramphenicol (CAP)) as a heterogeneous Fenton-like catalyst. The C/Fe3C/Fe0 composite demonstrated excellent performance for both OTC and CAP removal as compared with Fe0 and biochar. Furthermore, X-ray photoelectron spectrometry, Fourier transform infrared spectrometry, high performance liquid chromatography-mass spectra and electron spin resonance analyses were conducted to elucidate the adsorption and degradation mechanisms. The adsorption of OTC and CAP was mainly dominated by H bonds and the electron-acceptor-acceptor on the surface of the C/Fe3C/Fe0 composite, respectively. In particular, OH simultaneously induced the degradation of OTC and CAP, while 1O2 presented the selective oxidation to OTC. More specifically, the degradation of OTC over C/Fe3C/Fe0 was stronger and faster than that of CAP, leading to 65.84% and 16.84% of removal efficiency for OTC and CAP, respectively. Furthermore, C/Fe3C/Fe0 exhibited superior reusability and stability after regeneration, but regenerated Fe0 almost lost its reactivity. Therefore, the efficiency in situ generation of 1O2 using C/Fe3C/Fe0 would shed new light on the selective oxidation of aqueous organic compounds.

La2O3 media enhanced electrons transfer for improved CeVO4@halloysite nanotubes photocatalytic activity for removing tetracycline

Abstract A series of La2O3/CeVO4@halloysite nanotubes composites were successfully fabricated by the hydrothermal method. The La2O3/CeVO4@halloysite nanotubes composites display outstanding photocatalytic activity for removing tetracycline (TC) solution under visible light irradiation (λ ≥ 420 nm). After irradiation 60 min, an optimized La2O3/CeVO4@halloysite nanotube composite exhibited a high photocatalytic activity (87.1%), which is 3.89 times higher than that of raw CeVO4 (22.4%). The improvement of ternary composites performance is attributed to the Ce3+ and Ce4+ pairs in CeVO4. Besides, constructing heterojunctions between La2O3 and CeVO4 can inhibit the recombination of photoinduced electrons and holes, which is ascribed to the La3+ as electron trap to enhance the charge transfer. According to the trapper experiments and Electron Spin Resonance (ESR) analysis, the h+ and •O2− are major reactive species during the degradation. In addition, the oxygen vacancies are in the ternary photocatalyssts. The photocatalytic degradation intermediates of the solution were identified by High performance liquid chromatography-Mass spectra (HPLC-MS).

Homocysteine upregulates interleukin-17A expression via NSun2-mediated RNA methylation in T lymphocytes

Interleukin-17A (IL-17A) has been proven to participate in the process of various autoimmune diseases. The elevation of plasma homocysteine (Hcy), known as hyperhomocysteinemia (HHcy), is related to various chronic inflammatory diseases. Though HHcy-induced upregulation of IL-17A expression in T lymphocytes has been examined, the way in which IL-17A is regulated remains unclear. In this study, western blotting assays showed that Hcy (100 μM) upregulated NOP2/Sun domain family, member 2 (NSun2) expression in rat T lymphocytes. HHcy-induced upregulation of IL-17A observed in plasma of wild-type rats was markedly decreased in NSun2−/− rats in vivo. Mechanistically, by using in vitro methylation assays and high-performance liquid chromatography-mass spectrum (HPLC-MS) analysis, we showed that the tRNA methyltransferase NSun2 methylated the IL-17A mRNA in an m5C pattern. The results from bisulfite sequencing indicated that NSun2 methylated IL-17A mRNA at cytosine C466 in vitro and in vivo. Furthermore, we analyzed the activity of pGL3-derived reporters bearing IL-17A mRNA fragments and found that methylation by NSun2 promoted the translation of IL-17A. In conclusion, NSun2 mediates HHcy-induced upregulation of IL-17A expression by methylating IL-17A mRNA and promoting its translation in T lymphocytes.

Goethite promoted biodegradation of 2,4-dinitrophenol under nitrate reduction condition

Iron oxide may interact with other pollutants in the aquatic environments and further influence their toxicity, transport and fate. The current study was conducted to investigate the biodegradation of 2,4-dinitrophenol (2,4-DNP) in the presence of iron oxide of goethite under anoxic condition using nitrate as the electron acceptor. Experiment results showed that the degradation rate of 2,4-DNP was improved by goethite. High performance liquid chromatography-mass spectra analysis results showed that goethite promoted degradation and transformation of 2,4-diaminophenol and 2-amino-4-nitrophenol (2-nitro-4-aminophenol). Microbial community analysis results showed that the abundance of Actinobacteria, which have the potential ability to degrade PAHs, was increased when goethite was available. This might partially explain the higher degradation of 2,4-DNP. Furthermore, another bacterium of Desulfotomaculum reducens which could reduce soluble Fe(III) and nitrate was also increased. Results further confirmed that nanomaterials in the aquatic environment will influence the microbial community and further change the transformation process of toxic pollutants.

Analysis of Purified Oligomeric Proanthocyanidins from Larix gmelinii Bark and the Study of Physiological Activity of the Purified Product

A simple and efficient method for the purification of oligomeric proanthocyanidins (LOPC) from degreased Larix gmelinii bark was developed. The purity of LOPC was increased from 51.7% to 92.2%, and the cumulative recovery rate was 97.0%. The reversed phase high performance liquid chromatography-mass spectrum (RHPLC-MS) analysis indicated that the percentage contents of catechin (CA), epicatechin (EC), and procyanidin B1 (PB1) in purified LOPC (P-LOPC) were 5.05%, 2.02%, and 0.71%, respectively. The percentage contents of catechin and procyanidin B1 were noticeably higher than those obtained from grape seed extract (2.77% and 0.61%). The average degree of polymerization of P-LOPC was found to be 2.66. The matrix-assisted laser desorption ionization-time of flight/mass spectrum (MALDI-TOF/MS) analysis demonstrated that the dimer was the major component of purified LOPC and the distribution range was from dimer (m/z 713) to decamer (m/z 3016.6). The IC50 values of P-LOPC against DPPH• (1,1-diphenyl-2-picryl-hydrazyl), OH• (hydroxy radical), and ABTS+ (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid diammonium salt) were 76.4±3.82, 7.92±0.40, and 2.4±0.12. Purified LOPC exhibited more excellent physiological activity than VC (vitamin C), TBHQ (tert-butyl hydroquinone), and pine bark extract.

One-step green synthesis of bimetallic Fe/Pd nanoparticles used to degrade Orange II

To reduce cost and enhance reactivity, bimetallic Fe/Pd nanoparticles (NPs) were firstly synthesized using grape leaf aqueous extract to remove Orange II. Green synthesized bimetallic Fe/Pd NPs (98.0%) demonstrated a far higher ability to remove Orange II in 12h compared to Fe NPs (16.0%). Meanwhile, all precursors, e.g., grape leaf extract, Fe2+ and Pd2+, had no obvious effect on removing Orange II since less than 2.0% was removed. Kinetics study revealed that the removal rate fitted well to the pseudo-first-order reduction and pseudo-second-order adsorption model, meaning that removing Orange II via Fe/Pd NPs involved both adsorption and catalytic reduction. The remarkable stability of Fe/Pd NPs showed the potential application for removing azo dyes. Furthermore, Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) confirmed the changes in Fe/Pd NPs before and after reaction with Orange II. High Performance Liquid Chromatography–Mass Spectrum (HPLC–MS) identified the degraded products in the removal of Orange II, and finally a removal mechanism was proposed. This one-step strategy using grape leaf aqueous extract to synthesize Fe/Pd NPs is simple, cost-effective and environmentally benign, making possible the large-scale production of Fe/Pd NPs for field remediation.

Biodegradation of indole by a newly isolated Cupriavidus sp. SHE

Indole, a typical nitrogen heterocyclic aromatic pollutant, is extensively spread in industrial wastewater. Microbial degradation has been proven to be a feasible approach to remove indole, whereas the microbial resources are fairly limited. A bacterial strain designated as SHE was isolated and found to be an efficient indole degrader. It was identified as Cupriavidus sp. according to 16S rRNA gene analysis. Strain SHE could utilize indole as the sole carbon source and almost completely degrade 100mg/L of indole within 24hr. It still harbored relatively high indole degradation capacity within pH4–9 and temperature 25°C–35°C. Experiments also showed that some heavy metals such as Mn2+, Pb2+ and Co2+ did not pose severe inhibition on indole degradation. Based on high performance liquid chromatography–mass spectrum analysis, isatin was identified as a minor intermediate during the process of indole biodegradation. A major yellow product with m/z 265.0605 (C15H8N2O3) was generated and accumulated, suggesting a novel indole conversion pathway existed. Genome analysis of strain SHE indicated that there existed a rich set of oxidoreductases, which might be the key reason for the efficient degradation of indole. The robust degradation ability of strain SHE makes it a promising candidate for the treatment of indole containing wastewater.

Arabidopsis AtPAP1 transcription factor induces anthocyanin production in transgenic Taraxacum brevicorniculatum

This study developed a new purple coloured Taraxacum brevicorniculatum plant through genetic transformation using the Arabidopsis AtPAP1 gene, which overproduced anthocyanins in its vegetative tissues. Rubber-producing Taraxacum plants synthesise high-quality natural rubber (NR) in their roots and so are a promising alternative global source of this raw material. A major factor in its commercialization is the need for multipurpose exploitation of the whole plant. To add value to the aerial tissues, red/purple plants of the rubber-producing Taraxacum brevicorniculatum species were developed through heterologous expression of the production of anthocyanin pigment 1 (AtPAP1) transcription factor from Arabidopsis thaliana. The vegetative tissue of the transgenic plants showed an average of a 48-fold increase in total anthocyanin content over control levels, but with the exception of pigmentation, the transgenic plants were phenotypically comparable to controls and displayed similar growth vigor. Southern blot analysis confirmed that the AtPAP1 gene had been integrated into the genome of the high anthocyanin Taraxacum plants. The AtPAP1 expression levels were estimated by quantitative real-time PCR and were highly correlated with the levels of total anthocyanins in five independent transgenic lines. High levels of three cyanidin glycosides found in the purple plants were characterized by high performance liquid chromatography-mass spectrum analysis. The presence of NR was verified by NMR and infrared spectroscopy, and confirmed that NR biosynthesis had not been affected in the transgenic Taraxacum lines. In addition, other major phenylpropanoid products such as chlorogenic acid and quercetin glycosides were also enhanced in the transgenic Taraxacum. The red/purple transgenic Taraxacum lines described in this study would increase the future application of the species as a rubber-producing crop due to its additional health benefits.

The peripheral cannabinoid receptor 1 antagonist VD60 efficiently inhibits carbon tetrachloride-intoxicated hepatic fibrosis progression

This study investigated a peripheral selective CB₁ antagonist 3,4,22-3-demethoxycarbonyl-3-hydroxylmethyl-4-deacetyl-vindoline 3,4-thionocarbonate (VD60) that efficiently inhibited hepatic fibrosis with lower psychological side effects. A competitive radiolabeled ligand binding experiment and 3'-5'-cyclic adenosine monophosphate (cAMP) response element-driven luciferase analysis were performed to evaluate the antagonistic activity of VD60. Cell viability and collagen production were examined in the human hepatic stellate cell (HSC) line LX-2 and primary cultured rat HSCs. The antifibrotic effects of VD60 were investigated in a CCl₄-induced liver fibrosis mouse model. The concentration of VD60 in the blood and the brain was determined by high-performance liquid chromatography-mass spectrum analysis. Furthermore, the potential underlying mechanisms of VD60 were investigated by Western blot. VD60 selectively competed with the radiolabeled CB1 agonist to bind to CB1. VD60 antagonized CB1 agonist-induced Akt phosphorylation and increased the accumulation of intracellular cAMP. VD60 strongly reduced the expression of α₂(I) pro-collagen mRNA and exerted potent antiproliferative effects on primary HSCs and LX-2 cells. The inhibition of reactive oxygen species production and phosphorylation of Akt, extracellular-signal-regulated kinase (ERK), and Smad3 may explain the underlying mechanisms behind the antiproliferative effect of VD60. Moreover, the in vivo antifibrotic activity of VD60 was confirmed in a CCl4-induced liver fibrosis mouse model. Most importantly, the concentration of VD60 in the peripheral blood was much higher than in the brain, suggesting that VD60 could act as a novel peripheral CB1 antagonist to efficiently inhibit hepatic fibrosis and could be used as a lead compound with low brain side effects in peripheral antifibrotic agents.

Synthesis and Imaging Performance Research of a Ratio Fluorescent Dye for the Determination of Homocysteine/Cysteine in Living Cell

A Nile Blue based near-infrared fluorescent dye (RB-S) was reported, which was synthesized by a simple one-step reaction between 5-(dimethylamino)-2-nitrosophenol and 1-naphthaldehyde under mild reaction conditions. RB-S was well characterized using 1 H NMR, 13 C NMR, and TOF-MS. RB-S showed a significative fluorescent response to differ- ent concentrations of homocysteine or cysteine in the acetonitrile-water solution (4∶1, V/V, r.t.). Furthermore, with the con- centration of homocysteine or cysteine increasing, the fluorescent intensity of RB-S at 755 nm increased gradually, and that at 685 nm decreased. Exhilaratingly, there was a linear ratio fluorescent response (I755 nm/I685 nm) to the concentration of ho- mocysteine or cysteine in the range of 0.03~0.33 μmol/L. The recognition mechanism of the ratio fluorescent response to homocysteine or cysteine was verified by two experiment methods (high performance liquid chromatography-mass spectrum hyphenation technology and 1 H NMR titration) in this paper. A lot of detailed experiment results indicated that the ratio fluo- rescent response of RB-S to homocysteine or cysteine is most likely the result of the cyclization reaction of the aldehyde group to a thiazolidine group. The detection limit of RB-S for homocysteine or cysteine was determined as 0.025 μmol/L (3σ/k) in the acetonitrile-water solution (4∶1, V/V, r.t.). Besides sensitivity, the selectivity of RB-S for homocysteine or cys- teine was another very important parameter to evaluate in this paper. The selectivity experiments of RB-S were extended to 51 kinds of other biological-related species, including ion, amino acid and so on. All the experiment results demonstrated that RB-S was highly selective for homocysteine or cysteine over other related species and could meet the selective requirements for the fluorescent bioimaging and detecting of homocysteine or cysteine in vivo and in vitro. Therefore, RB-S was success- fully used to ratio fluorescent detect and image homocysteine or cysteine in serum samples and living cells by fluorescence spectrum and confocal fluorescence microscopic imaging, respectively. Keywords homocysteine/cysteine; fluorescent dye; Nile Blue; ratio; cell imaging

Hydroxyl radical induced by lipid in Maillard reaction model system promotes diet-derived Nε-carboxymethyllysine formation

N(ε)-carboxymethyllysine (CML) is commonly found in food, and is considered as a potential hazard to human health. However, the effect of lipids on CML formation in Maillard reaction is still not clarified. In this study, the content of diet-derived CML and its key intermediates, epsilon-fructoselysine (FL) and glyoxal (GO), is determined with high performance liquid chromatography mass spectrum (HPLC-MS) in model system containing lipid compounds. According to the results, hydroxyl radical (OH) induced by Fenton reagent can promote the three pathways of CML formation. Moreover, in the Maillard reaction system, linoleic acid (Lin), oleic acid (Ole) and glycerol trioleate (Tri) can induce more OH·, which promotes CML formation. Their level of promoting CML formation is in the order of Ole>Lin>Tri. On the contrary, glycerol (Gly) can scavenge OH·, which inhibit the CML formation. Finally, it is proved that FL content and GO content decreases with heating time in model system, while CML content increases with heating time. Thus, it is concluded that in the Maillard reaction system lipids can induce more OH·, which promotes the conversion from FL and GO to CML. Our research may contribute to the development of inhibitory methods for diet-derived CML by scavenging OH·.

Degradation of m-dihydroxybenzene by contact glow discharge electrolysis in aqueous

This paper reported the degradation of m-dihydroxybenzene aqueous solution with contact Glow Discharge Electrolysis. The rate of degradation in different conditions such as pH, H2O2, Fe2+, methanol, and other affecting factors were studied. The results showed that there is faster removal rate when the solution is in a relatively higher acidity; H2O2 can improve the efficiency rate. Fe2+ can promote reaction, but radical elimination agent of methanol will decrease the rate of the reaction. On the basis of analyzing the ultraviolet (UV) spectra of the solution and the intermediate products from High Performance Liquid Chromatography-Mass Spectrum (HPLC-MS), reaction pathway was proposed.

Photodegradation of amoxicillin by catalyzed Fe3+/H2O2 process

AbstractThree oxidation processes of UV-Fe3+ (EDTA)/H2O2 (UV: ultraviolet light; EDTA: ethylenediaminetetraacetic acid), UV-Fe3+/H2O2 and Fe3+/H2O2 were simultaneously investigated for the degradation of amoxicillin at pH 7.0. The results indicated that, 100% amoxicillin degradation and 81.9% chemical oxygen demand (CODCr) removal could be achieved in the UV-Fe3+ (EDTA)/H2O2 process. The treatment efficiency of amoxicillin and CODCr removal were found to decrease to 59.0% and 43.0% in the UV-Fe3+/H2O2 process; 39.6% and 31.3% in the Fe3+/H2O2 process. Moreover, the results of biodegradability (biological oxygen demand (BOD5)/CODCr ratio) revealed that the UV-Fe3+ (EDTA)/H2O2 process was a promising strategy to degrade amoxicillin as the biodegradability of the effluent was improved to 0.45, compared with the cases of UV-Fe3+/H2O2 (0.25) and Fe3+/H2O2 (0.10) processes. Therefore, it could be deduced that EDTA and UV light performed synergetic catalytic effect on the Fe3+/H2O2 process, enhancing the treatment efficiency. The degradation mechanisms were also investigated via UV-Vis spectra, and high performance liquid chromatography-mass spectra. The degradation pathway of amoxicillin was further proposed.

Rapid and high-throughput determination of cationic surfactants in environmental water samples by automated on-line polymer monolith microextraction coupled to high performance liquid chromatography–mass spectrometry

A rapid, high throughput and sensitive method was presented for automated determination of cationic surfactants in environmental water samples. The method was based on an automated analysis platform that was composed of on-line polymer monolith microextraction (PMME) and high performance liquid chromatography–mass spectrum (HPLC–MS) with an autosampler. A poly(methacrylic acid-co-ethylene dimethacrylate) (MAA-co-EDMA) monolith was selected as the sorbent for purification and enrichment of cationic surfactants in environmental water samples while a new mixed-mode chromatographic column packed with octyl and sulfonic acid co-bonded silica (OSS) was employed for separation and quantitative determination of cationic surfactants in water samples. By integrating sample preparation, chromatographic separation and MS detection into one automated platform, it makes the whole analysis procedure simple, accurate, and time and labor-saving. Several parameters affecting the extraction performance were investigated. Under the optimized conditions, the proposed method was applied to the analysis of seven cationic surfactants in environmental water samples. Good linearities were obtained for all cationic surfactants with R 2 larger than 0.9895. The limits of detection were found to be in the range of 15–24 ng/L. The method recoveries of the cationic surfactants spiked in water samples were from 80.5% to 115.1%, with relative standard deviations less than 12.4%.

Inhibiting JNK Dephosphorylation and Induction of Apoptosis by Novel Anticancer Agent NSC-741909 in Cancer Cells

NSC-741909 is a recently identified novel anticancer agent that suppresses the growth of several NCI-60 cancer cell lines with a unique anticancer spectrum. However, its molecular mechanisms remain unknown. To determine the molecular mechanisms of NSC-741909-induced antitumor activity, we analyzed the changes of 77 protein biomarkers in a sensitive lung cancer cell line after treatment with this compound by using reverse-phase protein microarray. The results showed that phosphorylation of mitogen-activated protein (MAP) kinases (P38 MAPK, ERK, and JNK) were persistently elevated by the treatment with NSC-741909. However, only the JNK-specific inhibitor SP600125 effectively blocked the apoptosis induced by NSC-741909. Moreover, NSC-741909-mediated apoptosis was also blocked by a dominant-negative JNK construct, suggesting that sustained activation of JNK is critical for the apoptosis induction. Further studies revealed that treatment with NSC-741909 suppressed dephosphorylation of JNK and the expression of MAPK phosphatase-1. Thus, NSC-741909-mediated inhibition of JNK dephosphorylation results in sustained JNK activation, which leads to apoptosis in cancer cells.