液-液萃取-气相色谱法测定水中9种有机氯农药   总被引：3，自引：1，他引：2  

王娜  王海娇  汪寅夫  李丽君 《岩矿测试》2010,29(5):497-502

采用正己烷液-液萃取法提取,气相色谱法-电子捕获检测器测定水中9种有机氯农药。优化了实验条件:添加两种替代物作为分析过程的质量监控;使用浓硫酸磺化法净化去除杂质;采用Rtx-5MS和Rtx-1701柱双柱定性,保证数据准确可靠。9种有机氯农药的方法检出限为0.0017～0.0079μg/L,回收率为74.7%～105.1%,相对标准偏差(RSD,n=7)为4.2%～9.3%,9种农药在0.5～100μg/L内与峰面积呈良好的线性关系。方法检出限低,准确度和精密度高,简便,适用于批量样品的分析。  相似文献   

成都锦江下游建立多级复合人工湿地净化污水的可行性研究     

孙遥  孙传敏  徐冠立 《四川地质学报》2011,31(1):67-70

锦江是成都市主要污水出口,黄龙溪镇出境断面水质为Ⅴ类或劣Ⅴ类水。本文对采用人工湿地处理锦江江水进行探讨,认为可以在锦江下游建立一系列多级复合人工湿地,湿地面积大约5～7km2,最终可使锦江出水达到Ⅲ类水域水质。  相似文献   

海洋放线菌ACMA006抗肿瘤活性成分的分离纯化及结构鉴定     

曹雪  杨瑞丽  袁献温  奚涛  杨臻峥 《台湾海峡》2011,30(3):400-404

对从中国江苏连云港海域中筛选出的海洋放线菌ACMA006的发酵产物进行了分离纯化,获得2种抗肿瘤活性化合物,并进一步鉴定其结构．海洋放线菌ACMA006经大规模发酵后,发酵液采用溶剂萃取法提取其中的抗肿瘤活性成分,并利用硅胶柱层析、制备薄层及HPLC等方法对萃取物进行分离得到单体化合物．利用红外光谱、质谱、核磁共振‘H—HMR谱和”C—NMR谱等波谱数据对单体化合物的结构进行解析和鉴定．结果表明化合物B为放线菌素D,其分子式为c62：H86N12016含有2个多肽酯环,由L一苏氨酸、D一缬氨酸、L．脯氨酸、N一甲基甘氨酸和L—N一甲基缬氨酸组成,通过羧基与发色母核吩唾嗪酮相连接．化合物A可能为放线菌素D的衍生物．这是国内外首次从海洋放线菌中分离提取出放线菌素D．  相似文献   

Studies on immunodiagnosis of hepatopancreatic parvo-like virus disease of the Chinese penaeid,Penaeus Chinensis I. Purification of the virus     

Sun Xiuqin  Wang Wenxing  Zhou Huimin  Zhang Jinxing  Xue Qinggang  Lu Ying  Song Qingyun 《中国海洋湖沼学报》1993,11(2):189-192

The viral discase of penaeids is indistinet but highly dangerous because their symptoms are often masked by some secondary ones. In order to gain knowledge on how to prevent the occurrence and spread of this viral disease, diagnostic studies on the early phase of the hepatopancreatic parvo-like viral (HPV) disease of culturedPenaeus chinensis was conducted using ummuno-serological techniques. The purification of HPV was successfully done by density gradient ultracentrifugation of cane sugar.  相似文献   

海洋沉积物中多氯联苯、多环芳烃和有机氯农药的同时净化与分离   总被引：4，自引：3，他引：1  

贺行良  夏宁  王江涛  张媛媛 《岩矿测试》2011,30(3):251-258

研究了海洋沉积物提取液中28种多氯联苯(PCBs)、16种多环芳烃(PAHs)和21种有机氯农药(OCPs)在硅胶-氧化铝复合净化柱上的同时净化与分离效果,结果表明:在充填4 cm3%去活化氧化铝-6 cm 3%去活化硅胶的8 mm i.d×15 cm固相萃取净化柱上,使用10 mL正己烷作为淋洗PCBs的分割点,可实现PCBs、PAHs和OCPs的满意分离,更有利于PCBs与高环数PAHs、极性较强OCPs的分离。继续用20 mL正己烷-二氯甲烷混合液(体积比1∶1)洗脱,28 PCBs、16种PAHs和21种OCPs均可获得有效回收,回收率分别为75%~110%、76%~115%、75%~130%。经海洋沉积物标准参考物质验证,该方法实用、可靠,流程简单,试剂消耗少,成本低,适用于海洋环境地质调查中基质复杂沉积物样品的定量分析。  相似文献   

软土地区提高旋挖钻机成孔质量的措施          下载免费PDF全文

王文明 《探矿工程》2013,40(9):68-71

针对某高架桥工程采用旋挖钻机在软土层钻进中发生的孔口坍塌、缩径、钻头打滑、孔底沉渣厚度大等情况,进行了原因分析,并采取了加长护筒、改进钻头结构、优化钻进工艺、气举反循环清孔、泥浆净化等针对性措施,取得了良好的效果,确保了工程质量,提高了施工效率,施工经验可供类似工程参考。  相似文献   

中国明对虾体壁N-乙酰-β-D-氨基葡萄糖苷酶的分离纯化及酶学性质     

林建城  林大河  林秀春 《海洋科学》2014,38(8):52-58

为了探讨对虾N-乙酰-β-D-氨基葡萄糖苷酶(EC3.2.1.52,NAGase)的分离纯化及其酶学性质,作者以中国明对虾(Fenneropenaeus chinensis)体壁为材料,通过硫酸铵沉淀分级分离、SephadexG-100柱层析和DEAE-32离子交换柱层析纯化,获得聚丙烯酰胺凝胶电泳纯的N-乙酰-β-D-氨基葡萄糖苷酶酶制剂,纯化酶比活力为3938.56U/mg。通过SDS-PAGE凝胶电泳,测得该酶亚基分子量为48.88 kD。酶的最适pH为6.0,最适温度为45℃;该酶在pH 6.0~9.0区域较稳定,温度稳定性范围是20~35℃,45℃下处理1 h酶活力丧失65.04%。酶水解对硝基苯-N-乙酰-β-D-氨基葡萄糖苷的Km为0.229 mmol/L,Vmax为5.00μmol/(L·min)。进一步研究金属离子对酶活力的影响,结果表明:Li+、Na+和Ba2+对酶没有明显影响,Mg2+、Ca2+、Mn2+、Co2+、Fe3+和Al3+对酶均有不同程度的激活作用,Cu2+、Zn2+和Pb2+对酶呈抑制作用,1.0 mmol/L Hg2+对酶呈激活作用,而10 mmol/L Hg2+使酶活力降低42.37%。  相似文献   

藤茶提取物中二氢杨梅素的化学纯化方法研究     

刘涛  张晓敏  郑红艳  万升标 《中国海洋大学学报(自然科学版)》2014,44(1)

藤茶粗提物含有二氢杨梅素和杨梅素等黄酮类化合物,其中以二氢杨梅素的含量最高。为从藤茶粗提物中分离得到纯的二氢杨梅素,本文选择用碘甲烷对藤茶提取物进行甲基化,柱色谱分离纯化得到五甲基化二氢杨梅素。用三溴化硼脱去甲基,得到纯的二氢杨梅素,产率为12.2%。二氢杨梅素结构经熔点、核磁共振氢谱、碳谱和质谱确认。  相似文献   

Purification and photodynamic bioactivity of phycoerythrin and phycocyanin from Porphyra yezoensis Ueda     

Chuner Cai  Yuan Wang  Chunxia Li  Ziye Guo  Rui Jia  Weining Wu  Yan Hu  Peimin He 《中国海洋大学学报(英文版)》2014,13(3):479-484

Phycoerythrin and phycocyanin were purified from Porphyra yezoensis Ueda with their bioactivity determined in this study. Continuous precipitation with ammonium sulfate at different concentrations （10%, 20%, 40%and 50%） increased the purity （A564：A280） of phycoerythrin to 1.49, 3.92 fold of the raw extract （0.38） and the purity （A615：A280） of phycocyanin to 0.70, 3.33 fold of the raw extract （0.21）. Two more times of chromatography with hydroxylapatites finally made the purity of phycoerythrin and phy-cocyanin reach 5.50, 14.47 fold of the raw extract, and 5.10, 24.29 fold of the raw extract, respectviely. The yield of high purity phycoerythrin and phycocyanin were 0.21%and 0.09%of dried P. yezoensis blade, respectively. The photodynamic cytotoxic ex-periment showed that both phycoerythrin and phycocyanin inhibited the growth of liver tumor cells significantly. It was found that 250 mg L-1 purified phycoerythrin and phycocyanin inhibited the growth of hepatocellular carcinoma cells 24 h after laser-irradiation by 80%and 59%, respectively, and 100 mg L-1 purified phycoerythrin and phycocyanin induced the apoptosis of 31.54%and 32.54%of the cells, respectively, 8 h after photodynamic therapy. Oue findings demonstrated that P. yezoensis can serve as photosensitizer （phycoerythrin and phycocyanin） producer.  相似文献   

Characterization of a bacteriocin-like substance produced from a novel isolated strain of Bacillus subtilis SLYY-3     

Junfeng Li  Hongfang Li  Yuanyuan Zhang  Xiaohui Duan  Jie Liu 《中国海洋大学学报(英文版)》2014,13(6):995-999

In the present research, the strain SLYY-3 was isolated from sediments of Jiaozhou Bay, Qingdao, China. The strain SLYY-3, which produced a bacteriocin-like substance(BLS), was characterized to be a strain of Bacillus subtillis by biochemical profiling and 16 S r DNA sequence analysis. It is the first time to report that Bacillus subtilis from Jiaozhou Bay sediments could produce a BLS. The BLS of B. subtillis SLYY-3 exhibited strong inhibitory activity against gram-positive bacteria(including Staphylococcus aureus and B. subtillis) and some fungi(including Penicillium glaucum, Aspergillus niger and Aspergillus flavus). The antimicrobial activity was detected from culture in the exponential growth phase and reached its maximum when culture entered into stationary growth phase. It was thermo-tolerant even when being kept at 100℃ for 60 min without losing any activity and stable over a wide p H range from 1.0 to 12.0 while being inactivated by proteolytic enzyme and trypsin, indicating the proteinaceous nature of the BLS. The BLS was purified by precipitation with hydrochloric acid(HCl) and gel filteration(Sephadex G-100). SDS-PAGE analysis of the extracellular peptides of SLYY-3 revealed a bacteriocin-like protein with a molecular mass of 66 k Da. Altogether, these characteristics indicate the potential of the BLS for food industry as a protection against pathogenic and spoilage microorganisms.  相似文献