微量穴醚(2.2.2)测定方法初探

用紫外分光光度法研究微量穴醚(2.2.2)的检测方法,并将该方法用于氟[18F]脱氧葡萄糖中微量穴醚(2.2.2)测定.将适量苯甲醛加入硝酸铅缓冲溶液中配制储备液,使溶液在250 nm检测波长处的吸收曲线为一平台,用储备液和微量穴醚(2.2.2)配制供试液,用紫外分光光度法检测.穴醚(2.2.2)的线性范围为1.0～10.0 μg/mL,相关系数0.999 5,平均回收率为100.5%(n=5),相对标准偏差为2.24%,方法检出限(3d)为0.15μg/mL.该方法用于氟[18F]脱氧葡萄糖中微量穴醚(2.2.2)测定,结果良好.该方法精密度高,准确性好,可用于微量穴醚(2.2.2)测定.

Abstract：

A method for the determination of trace cryptand 222 by ultraviolet spectrometry was researched. As benzaldehyde and complex of lead cryptand 222 possess the same ultralviolet absorbance peak and their maximum absorbance wavelength are both 250 nm, proper amount of benzaldehyde and lead nitrate was added to the citric acid buffer solution (pH=6.4) for preparing storage solution, and the ultralviolet absorbance curve of the storage solution was made a platform about 250 nm detection wavelength.Trace cryptand 222 was added to the storage solution, and trace complex of lead cryptand 222 was detected by ultraviolet spectrometry for quantitative determination of trace cryptand 222. This method kept in good linearity from 1.0 to 10.0 μg/mL of cryptand 222 concentration with a correlation coefficient of 0. 999 5, a recovery of 100.5% (n=5), a relative standard deviation of 2.24% and a limit of quantification of 0.15 μg/mL. This method has been successfully applied in determination of trace cryptand 222 of [18F]-fluorodeoxyglucose with satisfactory results. This method is simple, accurate and suitable for determination of trace cryptand 222.     

钯(Ⅱ)-盐酸吗啉胍螯合物与卤代荧光素染料相互作用的超瑞利散射光谱及其分析应用研究

在pH=4.4～5.0的HAc-NaAc介质中,钯(Ⅱ)与盐酸吗啉胍(Abob)反应形成螯合阳离子,它能进一步与二溴荧光素(DBF)、曙红Y(EY),赤藓红(Ery)阴离子反应形成离子缔合物,引起超瑞利散射(HRS)显著增强.3个三元体系具有相似的光谱特征,最大HRS波长位于390 nm附近.在一定条件下超瑞利散射增强(△IHRS)与Abob的浓度成正比,其线性范围是0.029～3.0μg/mL(DBF),0.14～3.5μg/mL(EY)和0.23～1.9μg/mL(Ery),检出限分别为0.008 6μg/mL(DBF),0.043 μg/mL(EY)和0.069μg/mL(Ery).研究了HRS法的适宜反应条件和共存物质的影响,发展了高灵敏、简便快速测定Abob的新方法,可用于尿样中Abob的测定.

Abstract：

In an acidic medium with pH = 4.4-5.0, palladium (Ⅱ) chelated with moroxydine hydrochloride to form the cation [ Pd (Abob)]2+ , which reacted further with dibromofluorescein (DBF), eosin Y (EY)and erythrosin(Ery) to form ion-association complexes, respectively. As a result, the hyper Rayleigh scattering(HRS) intensities were enhanced greatly. The maximum HRS peak of the three systems was all located at approximately 390 nm. HRS intensity was proportional to the concentration of moroxydine hydrochloride (Abob) in the range of 0. 029-3.0 μg/mL for DBF, 0. 14-3.5 μg/mL for EY and 0.23-1.9 μg/mL for Ery, and their detection limit (3σ) was 0. 008 6, 0. 043 and 0. 069μg/mL, respectively. The optimum conditions of the reaction and the properties of analytical chemistry were investigated. Therefore, a new method for the determination of moroxydine hydrochloride(Abob) by HRS was developed. The method has high sensitivity and good selectivity and has been applied to the determination of Abob in uric samples with satisfactory results.     

纳米微反应器化学发光法测定氢溴酸加兰他敏

在酸性条件下,氢溴酸加兰他敏被质子化后与AuCl4-形成离子缔合物被二氯甲烷所萃取,当缔合物被带入含鲁米诺的氯化十六烷基三甲基铵(Cetyltrimethylammonium Chlorine,CTAC)逆胶束纳米微反应器中时,离解出来的AuCl4-与鲁米诺产生化学发光.发光强度与氢溴酸加兰他敏的含量呈线性关系,从而可间接测定氢溴酸加兰他敏的含量.在优化的试验条件下,线性范围为0.001～15 μg/mL,检出限(3σ)为0.05 ng/mL,对浓度为1.0 μg/mL的氢溴酸加兰他敏进行11次平行测定,相对标准偏差(RSD)为2.24%.该法已成功用于片剂、针剂和生物体液中氢溴酸加兰他敏的测定.

Abstract：

Under the acidic condition, galantamine hydrobromide was protonated and formed an ion-complex with the negative ion AuCl4-, and the ion-complex was extracted by dichloromethane. When the ioncomplex entered a reversed micellar nanometer microreactor of cetyltrimethylammonium chlorine containing luminol, the dissociated AuCl4- reacted with luminol and produced an analytical chemiluminescnece signal. Under the optimum conditions, the CL response was linear to galantamine hydrobromide concentration ranging from 0. 001 to 15 g/mL and the limit of detection was 0.05 ng/mL with a relative standard deviation (n=11) of 2.24% for 1.0 g/mL galantamine hydrobromide. The method has been successfully applied to the determination of the studied drug in tablets, injections and biological fluids.     

流动注射抑制化学发光法测定阿魏酸

基于阿魏酸对鲁米诺-铁氰化钾化学发光体系的抑制作用,建立了阿魏酸的流动注射抑制化学发光分析法,在优化的实验条件下,阿魏酸浓度在4.0×10~(-7)～4.0×10~(-6) mol/L之间时,与化学发光强度减小值呈现良好线性关系,检出限为2.4×10~(-7) mol/L,对1.0×10~(-6) mol/L阿魏酸的相对标准偏差为1.4%(n=9),将其应用于复方当归注射液中阿魏酸含量的测定,结果令人满意.此外,结合化学发光光谱和紫外吸收光谱对抑制化学发光机理进行了初步探讨.

Abstract：

Based on the fact that the chemiluminescence intensity of the luminol- K3Fe(CN)6 system is inhibited in the presence of ferulic acid, a novel flow injection chemiluminescence inhibition method for the determination of ferulic acid was developed. Under the optimum conditions, the decrease in chemiluminescence intensity was linear with ferulic acid concentration in the range from 4. 0 × 10~(-7) to 4.0 × 10~(-6) mol/L.The detection limit was 2.4 × 10~(-7) mol/L and the relative standard deviation was 1.4% for 1.0 × 10~(-6) mol/L ferulic acid (n=9). When applied to the determination of ferulic acid in Fufang Danggui Injection samples, this method gave satisfactory results. Furthermore, combining the chemiluminescence spectra with the UV absorption spectra, the paper presents a brief discussion of their chemiluminescence inhibition mechanisms.     

The Determination of Canthaxanthin in Feed Ingredients by High Performance Liquid Chromatography

A series of studies were conducted to establish a methodology for the accurate and efficient determination of canthaxanthin in feed ingredients. Agilent ZORBAX Eclipse DB-C 18 analytical column （4.6×150 mm, 5μm） was used and kept at 25 ℃. The mobile phase was acetonitrile ： methanol （v/v）=95 ： 5, and eluted compounds were detected by DAD absorbance （470 nm）. The flow rate was maintained at 1.0 mL·min^-1. The response of the method was linear over the range 1.0-20.0 μg·mL^-1 canthaxanthin assay solution （R^2=0.9998）. Recovery assays done with standard canthaxanthin to feed ingredient resulted in an average recovery of 103%. Variation coefficient was less than 3.53%. This method is proved to be simple, precise, sensitive and reproductive.     

RP-HPLC同时测定口服液中的咖啡酸和阿魏酸

采用高效液相色谱法同时测定了口服液中的咖啡酸和阿魏酸含量,用Shim-pack VP-ODS柱(150 mm×4.6 mm,0.3μm),流动相:乙腈-3%的冰醋酸水溶液(体积比为11∶89),流速:1.0 mL/min,检测波长:321 nm.咖啡酸和阿魏酸的浓度与峰面积呈良好的线性关系,其线性范围分别为0.126～63.0 μg/mL(r=0.999 7)和0.120～24.0 μg/mL(r=0.999 9),平均回收率(n=3)分别为100.7%和99.9%,相对标准偏差(RSD)分别为2.11%和2.12%,检出限分别为42 ng/mL和43 ng/mL,样品中咖啡酸和阿魏酸的平均含量分别为3.26μg/mL和2.36μg/mL.

Abstract：

An HPLC method was established for the simultaneous determination of ferulic acid and caffeic acid in oral liquid. The Shim-pack VP-ODS column (150 mm×4.6 mm, 0.3 μm) was used with a mobile were detected at a wavelength of 321 nm. The flow rate was 1.0 mL/min and the injection volume was 20 μL. The calibration curve was linear in the range of 0. 126-63.0 μg/mL (r=0. 999 7) for caffeic acid and 0. 120-24.0 μg/mL (r=0. 999 9) for ferulic acid. The average recovery (n=3) was 100.7% with RSD 2. 11% for caffeic acid and was 99.9% with RSD 2.12% for ferulic acid. The detection limit was 42 ng/mL for caffeic acid and 43 ng/mL for ferulic acid. The average content of the samples was 3. 26 μg/mL for caffeic acid and 2.36 μg/mL for ferulic acid.     

Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

A fast analytical method for the simultaneous determination of 9 mycotoxins, including aflatoxins(B_1, B_2, G_1, and G_2), fumonisins(B_1, B_2 and B_3), zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-flight mass spectrometry(UPLC-Q-TOFMS) was developed and validated. Samples were extracted with acetonitrile-water(84:16, v:v, containing 1% acetic acid) using ultrasonic extraction. The extracts were purified with a dispersive SPE method using C18 as a cleaning agent. The final clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water(5:5, v:v). The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation(RSD) ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg~(-1), and limits of quantification ranged from 0.1 to 200 μg kg~(-1), which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, aflatoxins B_1 and fumonisins B_1, B_2 and B_3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×10~4, 0–6.94×10~3 and 0–3.05×10~3 μg kg~(–1), respectively.     

Rapid detection of Pseudomonas aeruginosa by cross priming amplification

Pseudomonas aeruginosa(PA) is an opportunistic pathogen of humans and animals and a common source of nosocomial infections especially of the respiratory tract. Pseudomonas aeruginosa is also a major bacterial disease of poultry and in particular, eggs and newly hatched chicks. In this study, we developed a simple, accurate and rapid molecular detection method using cross priming amplification(CPA) with a nucleic acid test strip to detect P. aeruginosa. The assay efficiently amplified the target gene within 45 min at 62°C only using a simple water bath. The detection limit of the method was 1.18×10~2 copies μL~(–1) for plasmid DNA and 4.4 CFU mL~(–1) for bacteria in pure culture, and was 100 times more sensitive than conventional PCR. We screened 83 clinical samples from yellow-feather broiler breeder chickens and hospitalized/treated dogs and cats using CPA, PCR and traditional culture methods. The positive-sample ratios were 15.3%(13/83) by CPA, 13.3%(11/83) by PCR and 12.1%(10/83) by the culture method. The established CPA method has significant advantages for detecting P. aeruginosa. The method is easy to use and possesses high specificity and sensitivity without the requirements of complicated experimental equipment. The PA-CPA assay is especially fit for outdoor and primary medical units and is an ideal system for the rapid detection and monitoring of P. aeruginosa.     

Effect of Agricultural Use of the Mixture Phosphogypsum/Natural Phosphate on the Dynamics of Phosphor in Soil and the Plant

The industrial production of the phosphoric acid is important and makes itself in a big number of countries. The by-product descended of this industry, residuary gypsum called phosphogypsum, poses a major environmental problem. The aim of this work is to identify and to value the potentialities of valorization of the by-product phosphogypsum produce in Morocco, for a use in the domain of agriculture. They can contain 1% to 6% of free acids. The idea is to use this acid to partially solubilize natural phosphate and to make the final product richer in phosphorus （about I0% of total P205 half soluble） and therefore more attractive on the agronomic and economic plan. For mixtures phosphogypsum/natural phosphate, a study of clarification is necessary, by varying the proportions of products, the humidities, mixing techniques, the ripening time to achieve a final interesting product. The dynamics of the phosphor in soil has been measured by the Olsen method and the one in the plant has been measured after drying in the steamroom to a temperature of 70 ~C to 75 ~C during 72 hours. A trial hold is incinerated. The ashes are taken by acid hydrochloric extract and the phosphor is measured out with the help of an UV spectrometer to 430 nm. The pH has been followed with the help of a pH-meter. The phosphor presents a remarkable dynamics in mixture with the phosphogypsum.     

Application of Current Hapten in the Production of Broad Specificity Antibodies Against Organophosphorus Pesticides

Diethylphosphono acetic acid （DPA） was used as a current hapten to generate broad specificity polycolonal antibodies against a group of organophosphorus pesticides. Six New Zealand white rabbits were immunized with immunogens synthesized by the active ester method （AEM） or 1-ethyl-3-（3-dimethylaminopropyl）-carbodimide method （EDC）. The titers of antisera reached 25 600 by AEM and 6 400 by EDC, respectively. Polyclonal antibodies raised against DPA were screened and selected for the competitive indirect enzyme-linked immunosorbent assay （CI-ELISA）. A CI-ELISA for DPA was developed with a detection limit of 3.536 ng mL^-1and an I50 value of 0.182 μg mL^-1. The assay specificity was evaluated by obtaining competitive curves for several structurally related compounds as competitors. The antiserum showed high affinities to chlorpyrifos, diazinon, omethoate, parathion-ethyl and profenofos with I50 of 0.12, 0.15, 0.21, 0.88, 0.97 and 2.5 μg mL^-1, respectively. The results indicate that the assay could be a screening tool for quantitation and semiquantitation determination of the above former five organophosphorus pesticides.