几丁糖酯原料药稳定性研究

该文建立高效凝胶渗透色谱法 (HPGPC) ,明胶比浊法 ,氧瓶燃烧法三种分析方法考察海洋硫酸多糖药物几丁糖酯的稳定性 ,采用这三种方法分别考察几丁糖酯原料药在高温、高湿、强光照射及加速条件下分子量及分布宽度、样品中硫酸根含量及样品含量的变化情况。结果表明 :三种方法均适用于几丁糖酯的稳定性考察 ,几丁糖酯在上述影响因素条件下稳定性良好     

6种鱼类肌肉组织肌苷酸的检测分析

采用高效液相色谱技术,在国内首次测定了条纹斑竹鲨(Chilocsyllium plagiosum)、大黄鱼(Pseudosci-aena crocea)、鳜(Siniperca chuatsi)、青石斑鱼(Epinephelus awoara)、牙鲆(Paralichthys olivaceus)和乌塘鳢(Bostrichthys sinensis)等6种鱼类新鲜和冻存肌肉组织中肌苷酸含量。结果表明:(1)不同鱼类肌肉组织中肌苷酸质量比不同,牙鲆新鲜肌肉组织中肌苷酸质量比最高,为4.214 mg/g,其余5种鱼类为2.365~3.634 mg/g。(2)10 d冻存试验中,经-70℃超低温冻存,6种鱼类冻存肌肉组织中肌苷酸质量比均高于新鲜肌肉组织,大黄鱼肌肉组织冻存1 d肌苷酸质量比达最大值,鳜肌肉组织冻存10 d肌苷酸质量比呈上升态势未出现最大值,其余5种鱼类肌肉组织肌苷酸质量比均在冻存第5天达到最大值。长时间的冻存将会降低食用鱼肉中肌苷酸质量比,导致鲜味下降,但经1周左右短时间的冻存后可明显提高鱼肉中肌苷酸质量比,增加鲜味,提高食用价值。     

An Acetic Acid‐Based Extraction Protocol for the Recovery of U,Th and Pb from Calcium Carbonates for U‐(Th)‐Pb Geochronology

A new method for the simultaneous recovery of U, Th and Pb from ca. 0.5 g calcium carbonate samples for the purpose of U‐(Th)‐Pb geochronometry is presented. The protocol employs ion‐exchange chromatography. Standard anion exchange resin (AG 1‐X8 100–200 mesh) was used as the static phase, and 90% acetic acid was used as the mobile phase to elute the unwanted matrix components; dilute nitric acid was used to elute the U, Th and Pb. Blanks of 1.8 pg Th, 6.4 pg Pb and 8.4 pg U were obtained. The protocol was evaluated by determining the isotopic composition of U‐Th‐Pb separates obtained from an in‐house reference material (prepared from a natural speleothem) by MC‐ICP‐MS. An independently dated speleothem was also reanalysed. Based on these tests, the extraction protocol had an acceptable blank and produced a Pb separate sufficiently free of matrix‐induced instrumental biases to be appropriate for U‐Th‐Pb chronology.     

Biodegradation Studies on Acid Violet 19, a Triphenylmethane Dye,by Pseudomonas aeruginosa BCH

Acid violet 19 (AV) belongs to the triphenylmethane (TPM) class of dyes which are potentially mutagenic or carcinogenic. However, very little studies on biodegradation of AV were reported as compared to other TPM dyes such as malachite green and crystal violet. In this study, AV was decolorized up to 98% within 30 min by Pseudomonas aeruginosa BCH. The decolorization depends on the initial dye concentration, pH, and temperature. However, the dye was decolorized under wide pH and temperature ranges with an optimum of pH 7 and 30°C. Up to 250 mg L^?1 of dye was found to be tolerated and decolorized by this strain. It showed decolorization ability for seven repeated dye addition cycles. The effect of additional carbon sources on dye decolorization was studied in which mannitol containing medium showed decolorization in 15 min. Induction in the enzyme activities of laccase, NADH‐DCIP reductase, and veratryl alcohol oxidase (VAO) indicates their involvement in AV degradation. Various analytical studies viz. UV–VIS, HPTLC, HPLC, and FTIR confirmed the biodegradation of AV by the bacterium. Based on GC‐MS analysis, a possible degradation pathway for AV was proposed. The phytotoxicity studies using Phaseolus mungo and Sorghum vulgare revealed the less toxic nature of metabolites formed after AV degradation.     

海洋细菌脂肪酸的气相色谱分析

以副溶血性弧菌VP-X-3为试验对象,利用气相色谱技术分析了其细胞脂肪酸的组成和含量,以色谱峰的数量、色谱峰高及脂肪酸含量作为评价指标,探讨了不同的皂化和甲酯化条件对细菌细胞脂肪酸测定结果的影响。结果表明:皂化和甲酯化条件都对细胞脂肪酸的组成和含量产生一定的影响。较低温度皂化处理利于增加色谱峰数量和色谱峰高。甲酯化温度过高容易破坏脂肪酸,尤其是长链脂肪酸和不饱和脂肪酸的结构。高温甲酯化条件下,时间越长,甲酯化效果越差。试验得到较为理想的气相色谱前处理条件:2 mol/L NaOH-甲醇溶液2 mL,70℃水浴10 min;10%(V/V)H2SO4-甲醇溶液2 mL,70℃水浴15 min。此条件下的色谱峰的数量多达29种,色谱峰高明显高于其他处理条件下的峰高。     

分散液液微萃取-气相色谱法测定环境水样中间甲苯酚

针对环境中痕量的间甲苯酚用一般仪器很难直接分析测定的问题,提出将分散液液微萃取技术与气相色谱联用测定环境水样中间甲苯酚的新方法.实验考察了影响分散液液微萃取效率的因素,包括萃取剂种类和用量、分散剂种类和用量、萃取时间、离心时间和盐度等,确定了最佳萃取条件为:200μL氯苯(萃取剂)和2.5mL丙酮(分散剂)混匀后,快速注入水样,室温静置8min,以3000r/min离心8rain,吸取1μL沉积相进行气相色谱分析.实验结果为:在最佳的萃取条件下,间甲苯酚的富集倍数为98.7倍,方法的线性范围为0.05～50mg/L,检出限为4.2μg/L(S/N=3),相对标准偏差为5.64％.将方法用于实际水样的测定,水样的加标回收率在86％～～122％,相对标准偏差(RSD)为3.3％～7.3％(n=3),实验表明该方法操作简便快速、成本低、环境友好,可用于实际水样的测定.     

Measurement of trace nitrate concentrations in seawater by ion chromatography with valve switching

An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix flowed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity （R〉0,99） in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability （RSD〈5%, n=6）. The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.     

地质勘探过程中煤层气联测氢气方法

瓦斯的危害和煤层气的利用,不断在推进着瓦斯地质理论、煤层气开发利用技术的进步和发展。在以往的诸多研究中,不论是防治瓦斯的危害还是着眼于煤层气的利用,甲烷都是研究的重点。但是,除甲烷之外,还有没有其它影响或控制瓦斯危害和煤层气利用的组分或因素呢？煤层气（瓦斯）联测氢气的方法和应用研究,就是循着这一思路而做的探索性工作。     

高效液相色谱-紫外光谱分析氢醌-双(β-羟乙基)醚

建立了高效液相色谱-紫外光谱法测定聚氨酯扩链剂氢醌-双(β-羟乙基)醚(HQEE)工业品中HQEE主含量和对苯二酚残留的方法。在氰基柱上,以甲醇-水-1%乙酸溶液(体积比10∶50∶40)为流动相,流速1.0 mL/min时,HQEE、对苯二酚及其他相关杂质得到良好分离,紫外光谱285 nm检测。方法简便、快捷,结果准确可靠,在工业生产中可有效地指导HQEE合成过程的质量控制。     

一种适用于沉积有机质族组分分离的微型柱色谱法

硅胶-氧化铝柱色谱是广泛采用的沉积有机质组分分离方法。但在常规柱色谱分离方法中,存在吸附剂、溶剂使用量过大、烷烃/芳烃组分交叉严重等问题。介绍一种微型柱色谱分离法,其分离效果与常规方法的效果基本相同或略有改善,吸附剂用量与样品的比例由100～250降低为25～50,洗脱溶剂与样品的比例由1800～4600降低至250～500。同时,操作程序进一步简化,分析成本和对环境的污染程度大幅度降低。