液-液相转移催化法合成N-芳氧基乙酰基-N′(2-氯苯甲酰基)肼

在液 液相转移催化条件下 ,以PEG 4 0 0为催化剂 ,通过芳氧基乙酰肼与 2 氯苯甲酰氯反应 ,合成了 10个尚未见文献报道的N 芳氧基乙酰基 N′ (2 氯苯甲酰基 )肼 .与经典方法相比 ,该法有操作简便 ,反应时间短 ,生产效率高等优点 .

不锈钢复合板生产方法和制备技术的探讨

介绍各种不锈钢复合板的生产方法和制备技术 ,着重分析了各种方法的优缺点和技术特点。同时介绍了几种正研究、开发中的新制备技术 ,展望了不锈钢复合方法的发展。

Stability of Baicalin Aqueous Solution by Validated RP-HPLC

Aim In the present study a RP-HPLC method was developed and validated toinvestigate the stability of baicalin aqueous solution. Methods The influences of temperature and pHon the stability of baicalin aqueous solution were investigated by classic homoiothermicacceleration test, and the pH for the most stable solution was determined. Results The time whenbaicalin suffered 10% loss was found to be 18.1 h, and the degradation activation energy of baicalinwas 79.1 kJ·moL^(-1) . The pH at which baicalin is most stable is 4.28. Conclusion The temperatureshould be kept at a lower level and the pH should be adjusted to near that for the most stablesolution in the production of baicalin preparations.

Determination of Candicidin/FR-008 and Related Components in Fermentation Broth by RP-HPLC

Aim A liquid chromatographic method for the determination ofcandicidin/FR-008 and related components in fermentation broth has been developed. Methods Therewere four major components in the candicidin/FR-008 complex, which were separated by HPLC under thefollowing conditions: SB-C8 column (4.6 mm x 250 mm, 5 μm) was used, the mobile phase consisted ofacetonitrileam-monium acteate (20 mmol·L^(-1) , pH 4.0) (40:60, V/V) , with a flow rate of 1 .0mL·min^(-1) , the UV detection wavelength was 380 nm, and the whole process was performed at 25℃ .Results The linearity was obtained in the range of 6.25 - 500 μg· mL^(-1) candicidin/FR-008 withthe regression equation of Y = 20 461 x + 30 748 and the correlation coefficient of 0.999 1. Theinstrument precision was 1.84% and the method precision was 3.8%. Conclusion This method isaccurate, rapid and simple; it can be used for determination of candicidin/FR-008 and relatedcomponents in fermentation broth.

Influences of the [Co^2＋]/[Co^3＋] Ratio on the Process of Liquid-phase Oxidation of Toluene by Air

Liquid phase oxidation of toluene is an environmental benign route for the production of benzoic acid.In a φ48mm bubble column reactor,the commercial process of toluene liquid phase oxidation was conducted with Co(CH3COO)2.4H2O as catalyst.The Co2+ concentration [Co2+] was determined by extraction spectrophotometry and hereby the Co3+ concentration [Co3+] was obtained by mass balance.The results showed that [Co3+] reached the maximum at about 25-30min.[Co3+] increased with increasing Co catalyst amount at total Co concentration<150 mg.L-1 of toluene.The conversion of toluene,yield and selectivity of benzoic acid increased with the increasing [Co3+/Co2+] max.A high [Co3+] and a high [Co3+]/[Co2+] ratio are beneficial to the reaction.

Liquid Chromatography-tandem Mass Spectrometry for Analysis of Acylcarnitines in Dried Blood Specimens Collected at Autopsy from Neonatal Intensive Care Unit

Objective To investigate the feasibility of analyzing acylcarnitine in dry filter-paper blood spots by liquid chromatography-tandem mass spectrometry(LC-MS/MS) which could be applied to detect inborn errors of metabolism in neonates.Methods We obtained filter-paper blood from 26 dead infants from a neonatal intensive care unit(NICU) between October 1,2008 and September 30,2009.Acylcarnitine and amino acid profiles were obtained with LC-MS/MS.Four infants underwent routine autopsy.The postmortem blood specimens were compared with newborn blood specimens,and with specimens obtained from older infants with metabolic disorders.Results Of all the 26 patients,5(19.2%) were diagnosed as having different kinds of diseases:3 with methylmalonic acidemia(the concentration of C3,and the ratio of C3/C16,C3/C2 increased),1 with maple syrup urine disease(the concentration of leucine and isoleucine increased),and 1 with isovaleric aci-demia(the concentration of C5 increased).Conclusions Postmortem metabolic test can explain infant deaths and provide estimates of deaths attributable to inborn errors of metabolism in NICU.LC-MS/MS is suitable for analysis of postmortem specimens and can be considered for routine application in NICU autopsy.

Changes of Metabolites and Macro- and Micro-elements in Hungarian Potatoes under Organic and Conventional Farming

To study the effect of cultivation system （conventional and organic） on potato tuber components, 42 parameters （anti-nutritives, micro- and macro-elements and 23 metabolites） were studied in three multi-resistant Hungarian potato varieties for three years in 2007-2009. Discriminant analysis of data proved that all investigated factors （farming technology, genotype and season/year） had significant effect on metabolites. Reversed phase high performance liquid chromatographic （HPLC-DAD, HPLC-MS） and elemental analysis methods have been adapted to quantify the major components, i.e., steroidal alkaloids, nitrite, nitrate, sugars, amino acids and micro-elements, in potato tubers. The absolute amount and changes of tuber components were influenced differentially by the technology, genotype and season in a complex manner. Any examined component, except nitrate content, was found to be significantly higher or lower consistently in relation to the production practice （organic or conventional） during the three years trials. Under the examined circumstances, no consequent positive effect of organic fanning on the total amount of anti-nutritive components, vitamins or micro- and macro-elements of potato tubers could be proven.

尼莫地平注射液光降解杂质定性研究

研究尼莫地平注射液经裸光照下主要的质量属性变化情况。有关物质表现为主要的特定降解杂质(尼莫地平杂质I)明显增加,同时产生较大的未知杂质RRT2.8。针对两个主要降解杂质,通过分析和推测杂质降解机理表明,尼莫地平杂质I增加与降解机理一致;并对新产生的降解杂质进行定性鉴别,采用液相色谱-质谱联用仪对该杂质进行一级质谱和二级质谱鉴别,推测出该杂质结构为尼莫地平杂质I二聚体,并通过实验分析该杂质降解途径,推测出该杂质降解机理。

碳酸锶纳米粉体的制备研究

以分析纯无水硝酸锶和碳酸钠为原料，在旋转填充床中采用液—液相法合成碳酸锶纳米粉体。其条件为：碳酸钠水溶液浓度０．５２５ ｍ ｏｌ／Ｌ，硝酸锶水溶液浓度０．５ ｍ ｏｌ／Ｌ，流量各６０ Ｌ／ｈ，转速０～１ ０００ ｒ／ｍ ｉｎ。得到平均粒径为３０ ｎｍ 的碳酸锶纳米粉体，粒度分布窄。该法过程简单，产率高，易于工业化。

A HPLC Method for the Determination of Salmon Calcitonin in Injection by Gradient Elution

It was concluded that the described HPLC method could be used for the assayof salmon calcitonin in injection, as it offers qualified selectivity, accuracy and precision ofanalysis.

Fucoxanthin Content of Five Species Brown Seaweed from Talango District, Madura Island

Fucoxanthin content of five brown seaweed species of East Java collected from Talango district （Madura sea-Jawa sea） namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargassum echinocarpum were determined and samples were collected using Global Positioning System （GPS）. Fucoxanthin from those samples was determined using Thin Layer Chromatography （TLC）, High Pressure Liquid Chromatography （HPLC） and Spectrophotometer UV-Vis and the results were then calculated using Seely equation. The pigments separation using HPLC gave a better result compared to TLC, and beside fucoxanthin otlher pigments namely chlorophyll and β carotene were also identified in these samples. Four points of sampling location were chosen using GPS and spot with coordinate positions observed were 113.94444° EL-7.08795° SA; 113.94231° EL-7.08913° SA. The results showed that fucoxanthin content were as follow： Padina australis 0.2674± 0.0046 mg/g; Turbinaria conoides 0.2134± 0.0100 mg/g; Sargassum filipendula 0.1957 ± 0.0173 mg/g; Sargassum cinereum 0.1640 ± 0.0092 mg/g and Sargassum echinocarpum 0.1576 ± 0.0001 mg/g. It can be concluded that Padina australis and Turbinaria conoides contain the most amount of fucoxanthin and it is possible to be cultivated as edible brown seaweed fucoxanthin resources.

Effects of temperature and phosphoric acid addition on the solubility of iron phosphate dihydrate in aqueous solutions

As important controlling factors for the synthesis of iron phosphate materials by liquid-phase precipitation, the solubilities of iron phosphate dihydrate were systematically measured at H3PO4 concentrations from 1.13 wt% to 10.7 wt% temperature from 298.15 to 363.15 K, and atmosphere pressure in this work. The solubility was found to increase 5 orders of magnitude or more with increasing the concentration of phosphoric acid, and de- crease 1 to 2 orders of magnitude with increasing the equilibrium temperature. The phosphoric acid addition and temperature were found to affect the solubility of iron phosphate dihydrate by the formation or dissociation of coordination species, which could further accelerate the phase transformation from the amorphous iron phosphate dihydrate to orthorhombic iron phosphate dehydrate by dissolution-recrystallization mechanism. The high dependences of the solubility of iron phosphate materials on HsPO4 concentration and temperature were also well predicted by calibration equations, which are meaningful for quantitatively understanding the precipitation process and sequential crystalline structure transformation and pursuing a rational strategy for syn- thesizing specific iron phosphate materials.

Persistence of malachite green and leucomalachite green in perch (Lateolabrax japonicus)

The persistence of malachite green (MG), and its metabolite leucomalachite green (LMG), in fish tissues is still unclear, leading to many trade disputes. In this research, we established and evaluated an HPLC method that could detect MG and LMG simultaneously, and then investigated the persistence of these two toxins in the tissues of juvenile perch (Lateolabrax japonicus) post sub-chronic MG exposure at 1.0 mg/L. Exposure lasted for 2 h everyday and was repeated six times. The perch were then placed in MG-free seawater for 100 d to eliminate the toxins. Results show that MG accumulated in the tissues, including the gills, liver, muscle, blood and viscera, and then was metabolized rapidly to LMG. The concentrations of these two toxins increased significantly with the accumulation process. In general, the highest concentrations of MG and LMG in all tissue exceeded 1 000 μg/kg, except for MG in the muscle. The order of accumulation levels (highest to lowest) of MG was gill>blood>liver>viscera>muscle, while that of LMG was liver>blood>gill>viscera>muscle. High levels of MG or LMG could persist for several hours but decreased rapidly during the elimination process. The concentration of LMG was much higher than that of MG during the experiment, especially in the gill, liver and blood. Therefore, the three tissues play important roles in toxin accumulation, biotransformation, and elimination. Although the MG and LMG concentrations in muscle were much lower than in other tissues, the content still exceeded the European minimum required performance limit (MRPL), even after 2 400 h (100 d) of elimination. This demonstrates that it is extremely difficult to eliminate MG and LMG from tissues of perch, and therefore use of these toxins is of concern to public health.

Economic and Qualitative Traits of Italian Alps Saffron

Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas.

Ultrafiltration of Shiitake Polyphenol with Ultrasound Enhancement

Ultrafiltration （UF） experiments were subjected to the concentration of Shi- itake polyphenol（SP） with ultrasound （US） enhancement, by which the effects of the main parameters such as ultrasonic power, transmembrane pressure, temperature and axial flow-rate on the membrane fluxes were analyzed, and then the SP of the ultrafiltrate after follow-up resin adsorption by HPLC was investigated. The results in- dicated that US could significantly enhance the membrane fluxes. The optimal con- ditions obtained was as follows： 0.60 W/cm2 US power, axial flow-rate of 80 L/h, operation temperature 30 ~C, transmembrane pressure 0.10 MPa. US increased the absorption capacity of the absorbent resin during the following stage. The HPLC analysis also showed that catechins were purified to some extent as the ultrafiltrate was treated by US and macroporous resin, indicating the technology of US en- hancement coupled with UF showed the potential for concentration and purification of SP by absorbent resins.

Removal of Pharmaceutically Active Compounds in Sequencing Batch Reactor

Biological treatment efficiency of six pharmaceutical compounds （acetazolamide, metronidazole, opipramol, piracetam, salicylamide and tinidazole） was evaluated using lab-scale Sequencing Batch Reactor （SBR）. Comparative biological degradation processes of two types of activated sludge from municipal and pharmaceutical industry sewage treatment plants were examined. Three different organic loadings （0.05 g COD/g MLSS.d, 0.1 g COD/g MLSS.d and 0.2 g COD/g MLSS-d） and reaction time on the efficiency of Active Pharmaceutical Ingredient （API） decomposition were examined. Chemical oxygen demand, non-purgeable organic carbon as well as ammonium nitrogen contents were monitored by standard methods. Percentage of API decomposition was analysed by High Performance Liquid Chromatography （HPLC）. The overall API removal efficiency was strictly dependent on the type of activated sludge origin. The main biodegradation products were identified using HPLC-MS,1H NMR and 13C NMR methods as e.g. （{4-[3-（5H-dibenzo[b,f]azepin-5-yl]piperazin-l-yl}methanamine） and （2-amino-1,3,4-thiadiazol-5-sulfonamide） for opipramol and acetazolamide respectively.

Production of Aflatoxins from Aspergillus flavus in Liquid Medium

Aflatoxins are produced mainly by Aspergillus flavus and Aspergillus parasiticus, and can be found in many grains such as peanuts, soybeans and com. This study aimed to qualitatively and quantitatively evaluate the production of aflatoxin in liquid media using strains of Aspergillus flavus obtained from peanuts marketed in the city of Fortaleza, CEo Strains of Aspergillus flavus were inoculated into a liquid medium malt extract and after 2 days inoculated into a second medium containing sucrose 5%, MgSO4·7H20 0.1%, KH2PO4 1%, ZnSO4·7H2O 0.0176 g, and cultured for 3 more days. The media were kept at room temperature ranging from 24°C to 32 °C with agitation of 130 rpm and aeration of 4.17 Llmin. Qualitative analysis was performed by thin layer chromatography and quantitatively by high performance liquid chromatography with fluorescence detection, demonstrating the production of aflatoxin B I （588 mg/L） and B2 （929 mg/L）.

Degradation of Antibiotics in Aqueous Solution by Photocatalytic Process： Comparing the Efficiency in the Use of ZnO or TiO2

The study examined the photodegradative efficiency of ZnO and TiO2 in degradation of antibiotics in aqueous matrices. Among several types of antibiotics, four antibiotics were chosen to feature the major classes of these compounds： amoxicillin, erythromycin, streptomycin and ciprofloxacin. Degradation of antibiotic solutions was carried out mainly under UV-light irradiation in a set time with the presence of small quantity of zinc oxide or titanium dioxide. Solutions were analyzed with HPLC chromatography and degradation percentages were calculated from ratio between pick area associated to no degraded drug solution and degraded drug solution＇s pick area. Meanwhile, toxicity of antibiotics and degrading compounds were investigated using a biosensor system, consisting of Clark＇s electrode associated with a portion of agar medium culture containing Saccharomyces Cerevisiae yeast cells. This way, it was possible to define the oxygen that was consumed by yeast cells. Toxicity associated to antibiotics and degrading products are related to decrease of oxygen concentration in solution. It is clear that zinc oxide is slower than titanium dioxide to degrade antibiotics, but zinc oxide shows better photodegradation efficiency than titanium dioxide in spite of its small specific superficial area.

Simultaneous determination of four nucleosides in Carthamus tinctorius L.and Safflower injection using high-performance liquid chromatography

We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid （TFA） aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL （r2= 0.9998）, 9.38-1407 μg/mL （rz = 0.9999）, 80.6-8060μg/mL （r2 = 0.9999） and 2.10---630μg/mL （r2 = 0.9987） with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.

Combination of dynamic hollow fiber liquid-phase microextraction with HPLC analysis for the determination of UV filters in cosmetic products

A simple method based on hollow fiber liquid-phase microextraction (HF-LPME) followed by high performance liquid chro-matography (HPLC) analysis was successfully developed for the determination of UV filters in cosmetic products. A canular extractor was assembled by mounting a hollow fiber inside an external tube with a tee-connector. The organic solvent was immobilized into the fiber to form a liquid membrane as the acceptor phase. The sample was continuously injected into the extractor and the UV filters were extracted from the aqueous sample into organic acceptor phase. The main parameters affecting HF-LPME including extraction solvent, sample volume, sample flow rate, pH values and ionic strength were investigated. Toluene has been verified to be suitable as the acceptor phase. Under the optimized HF-LPME conditions, the enrichment factors of five UV filters varying from 24 to 57 were achieved. The limits of detection for the five UV filters were in the range of 1-100 μg L-1 .The relative standard deviations (RSDs) of HF-LPME and HPLC analysis were lower than 5.2%. The proposed method has been successfully applied to the analysis of the varied cosmetic products.