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Methods Protein in blood and urine was precipitated directly by acetonitrile with acetanilide was used as the internal standard using Agilent Zorbax SB-Aq column (250 mm×4.6 mm, 5 μm). The mixed solvents of water (triethylamine 0.12%, acetic acid 0.12%) and acetonitrile were used as the mobile phase to separate cephalosporins using gradient elution method at 1 mL/min and 254 nm.

以乙酰苯胺为内标,血液和尿液用乙腈直接沉淀蛋白,采用Agilent Zorbax SB-Aq(250 mm×4.6 mm, 5 μm)色谱柱,流动相选用水(含0.12%三乙胺和0.12%乙酸)和乙腈的混合溶剂梯度洗脱,流速1 mL/min,检测波长254 nm。

After acidify with hydrochloric acid, the plasma was extracted with ethyl ether and then analyzed by Hypersil ODS2 (250×4.6 mm,5 μm) column with the mobile phase of methanol-water-triethylamine-acetic acid(2500∶1500∶15∶7), and at the detection wavelength of 355 nm.

血样经盐酸酸化后以乙醚提取,进行 HPL C分析,色谱柱为 Hypersil ODS2 (2 5 0× 4.6 m m,5 μm),流动相为甲醇-水-三乙胺-冰醋酸(2 5 0 0∶15 0 0∶ 15∶ 7)检测波长为 35 5 nm,尼美舒利为内标。

The aliquot was determined and confirmed by gas chromatography-negative chemical ionization mass spectrometry using external standard method.

样品中三唑醇残留物由正己烷饱和的乙腈(含1%冰醋酸)提取,加入无水硫酸镁与无水醋酸钠振荡促使提取液分层后进行固相分散萃取净化,用气相色谱-负化学离子源质谱法进行测定与确证,外标法定量。

The coal sample was combusted in the oxygen bomb containing ammonium carbonate solution and enough pressed oxygen.

在加有(NH4)2CO3溶液和过量氧气的氧弹中燃烧煤样,释放的氯被(NH4)2CO3溶液吸收,过滤溶液后,采用离子色谱外标法测定滤液中氯的浓度,最后计算出煤中氯的含量。

Methods: The method used direct sampling technique to determinate chloroform, bromodichloromethan, dibromochloromethane, bromoform, which was seperated by tube column, detected by electronic capture detector and determined by inner standard method.

水样直接进样,用毛细管柱色谱分离,电子捕获检测器检测,采用内标法定量,可同时测定水中三氯甲烷、一溴二氯甲烷、二溴一氯甲烷和溴仿。

First of all, internal standard method with HP-5 capillary column and SP-3420 chromatograph was established.

建立了对歧化反应产品进行气相色谱定量分析的内标法。

After washed, the chromogen substrate was added and incubated for 30 minutes in the dark. Rinsed with distilled water, purple spots were observed and counted using a dissection microscope. The number of spots means the level of cytokine producted by sCTL. Analysis of ability of specific cytotoxic lymphocytes to lyse target cells: CytoTox96 Non-Radioactive Cytotoxicity Assay kit was used.

5特异性CTL裂解靶细胞能力测定:采用CytoTox96 Non-RadioactiveCytotoxicity Assay试剂盒,将经HBV core18-27短肽、重组乙肝病毒核心抗原共刺激培养13日的PBMC与HLA-A2〓的靶细胞按一定比例混合,靶细胞被裂解后,释放的乳酸脱氢酶与底物反应显色,酶标仪测定吸光度,吸光度与裂解程度成正比,按照公式计算百分裂解率。

Column: Agilent C18; mobile phase 10mol.l-1 monobasic Acetate buffer, 20 molL-1triethylamine solution adjusted to pH5.5 with Acetic acid -acetonitrile ,gradient elution, flow rate: 0.6 mLmin-1; Results:The Traditional Chinese Medicines contained Acarbose, Phenformin and Glibenclamide, and can be separated completely.

色谱柱:Agilent ZORBAX ODS C18柱(5μm,4.6×250mm, Agilent);流动相:醋酸盐缓冲液(10molL-1醋酸胺,20 molL-1三乙胺,用醋酸调节pH5.5)与乙腈,梯度洗脱,流速:0.6 mLmin-1,色谱检测波长234nm,格列吡嗪为内标物进行定量分析。

Column: Agilent C18; mobile phase 10mol.l-1 monobasic Acetate buffer, 20 mol·L-1triethylamine solution adjusted to pH5.5 with Acetic acid -acetonitrile ,gradient elution, flow rate: 0.6 mL·min-1; Results:The Traditional Chinese Medicines contained Acarbose, Phenformin and Glibenclamide, and can be separated completely.

色谱柱:Agilent ZORBAX ODS C18柱(5μm,4.6×250mm, Agilent);流动相:醋酸盐缓冲液(10mol·L-1醋酸胺,20 mol·L-1三乙胺,用醋酸调节pH5.5)与乙腈,梯度洗脱,流速:0.6 mL·min-1,色谱检测波长234nm,格列吡嗪为内标物进行定量分析。

A method for simultaneous determination of oxytetracycline, tetracycline, chlortetracycline and choramphenicol in seafood was successfully developed using high performance liquid chromatography with ammonium acetate/water and acetonitrile as the mobile phase. The results showed that the four antibiotics were well separated under the optimum conditions, with the limits of detection being 32 μg/kg for oxytetracycline, 15 μg/kg for tetracycline, 23 μg/kg for chlortetracycline, and 19 μg/kg for choramphenicol. The recovery of standard additions was 76~92% and the relative standard deviation was 0.8-4.5%. The method is rapid, sensitive, accurate and reliable and can be applied in the analysis of antibiotic residues in seafood.

建立了同时检测海产品中土霉素、四环素、金霉素、氯霉素残留的高效液相色谱分析方法,以醋酸铵-醋酸/水缓冲液和乙腈作为流动相,通过二元梯度洗脱,使四种抗生素获得了较好的分离,以基线噪音的3倍计算,土霉素、四环素、金霉素、氯霉素最低检出浓度分别为32μg/kg、15μg/kg、23μg/kg、19μg/kg,在添加浓度范围内,四种抗生素的加标回收率为76~92%,相对标准偏差为0.8~4.5%,该方法快速、灵敏、准确,可靠性高,可用于海产品中抗生素残留的色谱分析。

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