Rapid liquid chromatographic analysis of Metoclopramide in pharmaceutical preparations

A sensitive, accurate and reproducible method for the analysis of metoclopramide, a gastrointestinal drug, has been described. An isocratic HPLC elution method was employed which requires about 10 minutes to be performed. The concentration of metoclopramide hydrochloride preparations was found to be 95.1 ±0.3% and 94.21 ±0.25% in tablet and injection formulations, respectively.     

3,3'-二氯联苯胺盐酸盐合成工业酸性废水中污染物的高效液相色谱法测定

利用高效液相色谱法测定了３,３’－二氯联苯胺盐酸盐合成工业酸性废水中的污染物,色谱柱为Ｚｏｒｂａｘ－ＯＤＳ,流动相为乙腈－水(７０/３０,Ｖ/Ｖ),流速为０．５ｍｌ·ｍｉｎ－１,柱温４２℃,检测波长２８０ｎｍ．建立了废水水样预处理方法,主要污染物回收率在９０%以上．酸性废水中污染物包括３,３'－二氯联苯胺盐酸盐、邻氯苯胺等．     

盐酸小檗碱对小鼠脾细胞的DNA损伤和氧化性损伤研究

为了探讨盐酸小檗碱对小鼠的DNA损伤和氧化性损伤。随机选取30只小鼠分成对照组以及7.5,15,30,60与120 mg?kg^-1实验组,处理后,应用小鼠脾细胞进行彗星实验与抗氧化酶实验。测定DNA损伤情况以及超氧化物歧化酶（SOD）、过氧化氢酶（CAT）、过氧化物酶（POD）活性以及丙二醛（MDA）含量变化。对盐酸小檗碱的DNA损伤与氧化性损伤作用进行比较研究。研究结果表明：彗星实验中,随着盐酸小檗碱浓度的增加,尾部DNA含量、尾长与尾矩均增加,与阴性对照组相比差异有统计学意义（p<0.05或p<0.01）,且呈剂量-效应关系;超氧化物歧化酶(SOD)与过氧化氢酶(CAT)活性随盐酸小檗碱剂量增加逐渐降低,丙二醛(MDA)含量明显下降,过氧化物酶(POD)活性在7.5 mg?kg^-1时上升,而后逐渐下降。在60 mg?kg^-1和120 mg?kg^-1时,有极显著性差异（p<0.01）产生。由此可见,盐酸小檗碱对小鼠脾细胞有一定的损伤作用,能够引起小鼠脾细胞的DNA损伤和氧化性损伤。     

盐酸胍诱导的apo-CP43去折叠过程

膜蛋白生物合成与色素组装中蛋白的稳定性可以通过去折叠条件与过程分析得到.利用色氨酸荧光光谱和ANS荧光光谱研究了apo-CP43在盐酸胍条件下的稳定性.色氨酸荧光光谱观测到apo-CP43在盐酸胍作用下去折叠进程的主要特征:荧光强度先是逐渐降低,之后再逐渐升高,而最大荧光发射峰位置则一直持续红移.盐酸胍处理后apo-CP43的F360 nm/F335 nm比值逐渐增大,表明荧光最大发射峰逐步红移.当盐酸胍浓度约为5.5 mol/L时,去折叠比例趋于相对稳定状态,说明此时apo-CP43已经基本完成去折叠.荧光相图法结果显示盐酸胍诱导apo-CP43变性的过程符合三态模型.ANS荧光测定数据显示盐酸胍处理之后最大ANS荧光发射峰位置红移,并且荧光强度逐渐降低.以上数据表明在盐酸胍条件下apo-CP43是一个相对比较稳定的蛋白.     

Tetracycline as a fluorescent shell-marker in the abalone Haliotis iris

Ageing of abalone by counting rings laid down internally in the shell has presented problems of validation. Three methods of tetracycline marking were tested in Haliotis iris. Juvenile (<70 mm shell length) and adult (>115 mm) abalone were injected intramuscularly with tetracycline hydrochloride, injected with oxytetracycline, or immersed in tetracycline hydrochloride. After treatment, shells were cut sagitally and examined under ultraviolet light using a stereomicroscope. In treatments where juveniles were injected with tetracycline hydrochloride or oxytetracycline hydrochloride at dosages ranging from 20 to 600 mg per kg body weight, no fluorescent marks were visible from treatments80 mg/kg, but 83% of juveniles treated with greater dosages retained a visible mark. In treatments where juveniles were immersed in seawater solutions of tetracycline hydrochloride at five concentrations ranging from 200 to 1000 mg per litre of seawater and sampled at 5 h intervals for periods ranging from 5 to 40 h, all showed clear fluorescent markings. Shells of adult abalone injected with tetracycline hydrochloride at four dosages ranging from 200 to 800 mg/kg all showed clearly visible marks 18 d post-treatment. Abalone injected at dosages of 600 and 800 mg/kg exhibited tissue fluorescence around the injection site 2 wk after treatment. Adults immersed for 48 h at four concentrations ranging from 200 to 800 mg/l produced marks comparable to those of injected adults. Abalone were clearly stressed by some treatments. Only 50% of adults injected at 200 mg/kg were able to right themselves within 10 min, while all those injected at higher concentrations either were incapable of righting themselves after treatment or were extremely sluggish. All immersed adults quickly righted themselves. These results show that both injection and immersion are effective in marking abalone, but that immersion is less stressful to them.     

甲醛对大鼠肺细胞醛糖还原酶的影响及醛糖还原酶功能研究

为了研究甲醛作用后大鼠肺细胞醛糖还原酶(AR)的活性变化以及AR在肺细胞损伤中的功能,首先通过大鼠肺细胞分离培养,观察甲醛对大鼠肺细胞AR活性的影响及AR抑制剂——盐酸小檗碱对AR活性的抑制作用;其次通过流式细胞仪检测甲醛及盐酸小檗碱对大鼠肺细胞周期和凋亡的影响.结果表明:1.0mmol·L-1甲醛作用24h使大鼠肺细胞AR活性显著增加,盐酸小檗碱对AR活性具有抑制作用;甲醛能够引起大鼠肺细胞凋亡,使G0/G1和S期的细胞比例下降,G2/M期的细胞比例增加;甲醛和盐酸小檗碱共同作用使大鼠肺细胞凋亡率较单纯甲醛组更高,同时G0/G1期的细胞比例增加,S和G2/M期的细胞比例下降.结果提示甲醛能够使大鼠肺细胞AR活性增加;AR活性增加可减少细胞凋亡,对甲醛引起的大鼠肺细胞损伤具有保护作用.     

Influence of insecticidal derivative (cartap hydrochloride) from the marine polycheate on certain enzyme systems of the fresh water fish Oreochromis mossambicus

The activities of phosphatases and transaminases were studied in muscle and liver of the fresh water fish, Oreochromis mossambicus on exposure to different sublethal concentrations (0.25, 0.5, 0.75 and 1 mgl(-1)) of cartap hydrochloride (insecticidal derivative from marine polycheate) for 96 h. There was an overall decrease in phosphatases and transaminases activity in muscle and liver of the fish subjected to cartap hydrochloride.     

Comparative account of certain enzymes in the serum of homo-iothermal vertebrates subjected to production of myocardial infarction by isoproterenol hydrochloride

Myocardial infarction was produced by subcutaneous administration of isoproterenol hydrochloride (85 mg/kg b.w. for two consecutive days). The myocardial damage was proved by observing increase in the activity of SGOT and SGPT in serum whereas AChE activity was inhibited by increasing Km, without affecting Vmax. The inhibition of AChE and inhibitory kinetic may be useful in the diagnosis and management of salvage of myocardium.     

Development of a complex-based flow injection spectrophotometric method for determination of the herbicide pinoxaden in environmental samples

A flow injection (FI) spectrophotometric method for the determination of the herbicide pinoxaden (PXD) has been proposed. PXD was converted in alkaline media with hydroxylamine hydrochloride to the hydroxamate salt. The salt was reacted with iron(III) chloride, and the absorbance of the red colored tris iron hydroxamate complex was measured at 500?nm using a FI system. The method was found to be linear between 0.5 and 40?mg?L^?1 with a molar absorptivity of 1.53?×?10^4?L?mol^?1?cm^?1. The limit of detection and limit of quantification were found to be 0.1?±?0.01?mg?L^?1 and 0.6?±?0.05?mg?L^?1, respectively. Any interference of fenoxaprop-p-ethyl (FE) was avoided by the separation of PXD by liquid chromatography with a mixture of dichloromethane and n-hexane (1?:?1) as eluent. The method was applied to the determination of PXD in soil, water, and wheat grains with percent recoveries of 98?±?2, 100?±?2, and 98?±?5, respectively. Sample throughput of 60 samples per hour was achieved under optimized conditions.     

土壤和沉积物中的聚合有机质对多环芳烃分布和提取的影响

为了研究土壤和沉积物中凝聚型有机碳(碳黑、干酪根)的含量及其对多环芳烃(PAHs)分布和提取的影响,分别用三氟醋酸(TFA)和在375℃下通氧燃烧的方法从珠江三角洲2个污染土壤和5个河口沉积物样品中提取酸非水解有机碳(NHC)和碳黑(BC);用索氏抽提法和不同溶剂的加速溶剂萃取法(包括连续加速萃取法ASESum和标准溶剂萃取法ASESTD)抽提土壤和沉积物中的多环芳烃,并在不同温度梯度(25℃到150℃)下用水为溶剂加速溶剂萃取其水溶态.结果表明,1)NHC是珠江三角洲土壤和沉积物中总有机碳的重要组成部分,NHC碳明显高于BC碳,NHC和BC分别占土壤和沉积物中有机碳的25.6%￣73.8%和4.64%￣17.3%.2)3种有机溶剂(丙酮、甲苯1、甲苯2)连续抽提的PAHs含量是索氏抽提的2.11倍;5种ASE方法(丙酮、甲苯1、甲苯2、ASESum、ASESTD)提取的PAHs含量与NHC含量存在明显的相关性,而且比PAHs含量与BC或无定型有机碳(AOC)含量的相关性更明显.3)在不同温度梯度下水溶态PAHs浓度符合Van’tHoff方程.研究说明除了BC外,非水解有机碳对土壤和沉积物中PAHs的分布和提取具有重要影响.     

六方水钠锰矿对罗丹明B的去除效果及机理

六方水钠锰矿作为环境中一种具有较强氧化与吸附能力的氧化锰矿物,对环境中的有机染料有着一定的去除作用.采用常压回流法一步合成纳米六方水钠锰矿,运用X射线衍射(XRD)、电感耦合等离子体光谱仪(ICP-AES)、BET氮气吸附法、场发射扫描电镜(FESEM)和透射电镜(TEM)对其矿物晶体结构、化学组成、比表面积、孔径分布...     

Photolytic decomposition of uc‐54229, a Proinsecticide of the Carbamate group

Phototransformation of UC‐54229 (1) [2,3‐dihydro‐2,2‐dimethyl‐7‐benzofuranyl‐N‐(trimethylamino acetyl)‐N‐methyl carbamate chloride] was studied under UV and visible light conditions. Photoirradiation of 1 with UV‐light resulted in the formation of five degradation products which on the basis of their mass and ¹H Nmr spectral analysis were characterised as 2, 3, 4, 5 and 6. It was observed that under the influence of light, UC‐54229 was degraded to acetyl‐carbofuran which under similar conditions underwent further transformation to the actual toxicant carbofuran. The degradation products or impurities present in 100% water soluble powder formulation were identified as carbofuran phenol and triethylamine hydrochloride.     

Fabrication of highly efficient Bi2WO6/CuS composite for visible-light photocatalytic removal of organic pollutants and Cr(VI) from wastewater

• A novel Bi₂WO₆/CuS composite was fabricated by a facile solvothermal method. • This composite efficiently removed organic pollutants and Cr(VI) by photocatalysis. • The DOM could promoted synchronous removal of organic pollutants and Cr(VI). • This composite could be applied at a wide pH range in photocatalytic reactions. • Possible photocatalytic mechanisms of organic pollutants and Cr(VI) were proposed. A visible-light-driven Bi₂WO₆/CuS p-n heterojunction was fabricated using an easy solvothermal method. The Bi₂WO₆/CuS exhibited high photocatalytic activity in a mixed system containing rhodamine B (RhB), tetracycline hydrochloride (TCH), and Cr (VI) under natural conditions. Approximately 98.8% of the RhB (10 mg/L), 87.6% of the TCH (10 mg/L) and 95.1% of the Cr(VI) (15 mg/L) were simultaneously removed from a mixed solution within 105 min. The removal efficiencies of TCH and Cr(VI) increased by 12.9% and 20.4%, respectively, in the mixed solution, compared with the single solutions. This is mainly ascribed to the simultaneous consumption electrons and holes, which increases the amount of excited electrons/holes and enhances the separation efficiency of photogenerated electrons and holes. Bi₂WO₆/CuS can be applied over a wide pH range (2–6) with strong photocatalytic activity for RhB, TCH and Cr(VI). Coexisiting dissolved organic matter in the solution significantly promoted the removal of TCH (from 74.7% to 87.2%) and Cr(VI) (from 75.7% to 99.9%) because it accelerated the separation of electrons and holes by consuming holes as an electron acceptor. Removal mechanisms of RhB, TCH, and Cr(VI) were proposed, Bi₂WO₆/CuS was formed into a p-n heterojunction to efficiently separate and transfer photoelectrons and holes so as to drive photocatalytic reactions. Specifically, when reducing pollutants (e.g., TCH) and oxidizing pollutants (e.g., Cr(VI)) coexist in wastewater, the p-n heterojunction in Bi₂WO₆/CuS acts as a “bridge” to shorten the electron transport and thus simultaneously increase the removal efficiencies of both types of pollutants.     

单甲脒等农药的土壤薄层层析行为

用土壤薄层层析法研究单甲脒，单甲脒盐酸盐、灭幼脲和涕灭威等农药在不同土壤中的迁移行为，分别获得了这几种化合物的Ｒｆ值，它们分别为０．１４、０．１７，０．０８，０．７６，研究表明，单脒，单甲脒盐酸盐和灭幼脲不会污染地下水，而涕灭威则会对地下水污染构成严重的威胁。     

Removal and recovery of uranium(VI) by adsorption onto a lignocellulosic-based polymeric adsorbent containing amidoxime chelating functional group

A new adsorbent (ABS) with amidoxime functional group was prepared through graft polymerization of acrylonitrile onto banana stem (BS) using ceric ammonium nitrate (CAN)/HNO₃ initiator system, followed by treatment with hydroxylamine hydrochloride in alkaline solution. Infrared spectroscopy, surface area analyzer, thermogravimetry, and potentiometric titration were used for the characterization of the adsorbent. Effective removal of U(VI) ions was demonstrated at the pH range 4.0–6.0. The mechanism for the removal of U(VI) ions by ABS was based on complexation adsorption model. Equilibrium was achieved in approximately 3 h. The experimental kinetic data were analyzed using first-order, second-order, and Elovich kinetic models, and are well fitted with second-order kinetics. The temperature dependence indicates an exothermic process. U(VI) adsorption was found to decrease with increase of ionic strength. The Freundlich isotherm model fitted the experimental equilibrium data well. The adsorption efficiency was tested using synthetic nuclear industry effluents. The maximum adsorption capacity for U(VI) removal was found to be 80 mg g^-1 at 20°C. Adsorbed U(VI) ions were desorbed effectively, about 99% by 0.2 M HCl. Repeated adsorption/desorption cycles show the feasibility of the ABS for the removal of U(VI) ions from water and nuclear industry effluents.     

磺胺和四环素类抗生素对大肠杆菌联合突变效应的研究

抗生素的滥用造成的环境安全问题已不可忽视,关于抗生素联合毒性效应研究较多,但联合突变效应研究较少。因此,本文以大肠杆菌为受试生物,研究了2种磺胺类抗生素(磺胺氯哒嗪(SCP)、磺胺二甲嘧啶(SMZ))和3种四环素类抗生素(二甲胺四环素(MH)、盐酸四环素(TH)和盐酸强力霉素(DH))单一及联合暴露时对大肠杆菌的突变效应。结果表明:在单一暴露下,磺胺类抗生素会促进大肠杆菌的突变效应,四环素类抗生素没有明显的促进作用;联合暴露下,磺胺类抗生素对大肠杆菌突变效应为相加,磺胺和四环素类抗生素对大肠杆菌突变效应为拮抗。本研究初步探索了抗生素对大肠杆菌的联合致突变风险,为今后环境中抗生素混合暴露的生态风险评价和抗生素污染控制标准制定提供一种理论支撑。     

Estimating the uncertainty of pesticide residue analysis from mango using multi-residue analysis and validation of method

Validation of method was performed for various pesticides on mango matrix involving the processing of sample at ambient and cryogenic conditions. The linearity, limits of detection, repeatability, matrix effect, and recovery were studied as the aspects of method validation. The effect of matrix on recovery was found to be medium (20–50%) and strong (>50%). After correction by matrix-matched calibration curves, the recovery was calculated to be in the range of 80–107% and 80–105% at ambient and cryogenic processing, respectively. The precision estimated for the recovery of pesticides obtained from both solvent- and matrix-matched calibration curves and at both the processing conditions was determined to be >20% except for chlorpyrifos and atrazine. The uncertainty established for the methodology was >20%, which substantiates the efficiency and reliability of methodology used for pesticide residue analysis in mango in this study.     

GC-MS-MS测定蔬菜中八种有机磷农药

用GC-MS-MS同时测定蔬菜中的甲拌磷、二嗪农、甲基对硫磷、毒死蜱、倍硫磷、喹硫磷、杀扑磷和亚胺硫磷.对各个化合物的特征离子对、碰撞电压进行了优化,并阐述了优化反应监测模式(MRM)条件的过程和方法,同时分析了各个化合物的线性范围和最低检出限.将该方法用于蔬菜样品的检测,测得加标回收率在90.4%-105.0%之间,RSD在3.2%-9.3%之间.     

Toxic effect assessment of aminotetrazoles and high-energetic azotetrazole salts on soil microbial respiration

The influence of energetic heterocyclic high-nitrogen salts on microbial activity in soil enrichment was investigated. 5-Aminotetrazole, a sodium salt of 5-aminotetrazole, ammonium azotetrazolate, sodium azotetrazolate, guanidinium azotetrazolate, triaminoguanidine azotetrazolate and triaminoguanidine hydrochloride were examined. Respiration tests determined the amount and rate of production of CO₂, H₂ and H₂S from microbial activity. Aminotetrazoles, triaminoguanidine azotetrazolate and triaminoguanidine hydrochloride substantially reduced the amount and rate of microbial CO₂ production. The total amount of CO₂ produced in the soil enrichments was affected by the cation from the azotetrazole salt, whereas the azotetrazolate anion did not seem to inhibit microbial CO₂ production. In contrast, all applied compounds stopped the production of H₂S completely and modified the rate of H₂ production in the cultures compared with the control. The influence of ammonium azotetrazolate and sodium azotetrazolate on the activity of isolated sulfate-reducing bacteria was also determined. The compounds did not have bactericidal activity towards sulfate-reducing bacteria, but the compounds decreased the amount of H₂S produced or slowed the growth of these bacteria in comparison with the control.     

Exploring the mechanism of ammonium uptake in phytoplankton with an ammonium analogue,methylamine

Uptake of the ammonium analogue methylamine hydrochloride was used to examine the mechanism of ammonium transport in several species of marine phytoplankton (mainly Skeletonema costatum, but also Thalassiosira weissflogii, Emiliania huxleyi and Gonyaulax polyedra). Ambient pH had no effect on the retention of methylamine between pH 3.6 to 9.2 HgCl₂ markedly inhibited methylamine transport. Transport was temperature-dependent and the Michaelis-Menten equation described methylamine transport as a function of concentration in experiments of less then 20 to 30 min duration. Pulse-chase experiments showed that only 5 to 15% of intracellular methylamine was readily exchanged with external methylamine or ammonium, and the remaining 85 to 95% exchanged more slowly. These results suggest that methylamine transport, hence ammonium uptake, probably was an active metabolic process as it occurred against typical values of algal electrochemical gradients. The acid-trap model of ammonium transport was not consistent with these data. A two-compartment model where ammonium is transported into the cytoplasm and vacuole is proposed.