依替米星在不同溶媒中的稳定性研究

实验采用HPLC法,以C18柱为色谱柱,CH3OH：H2O：HAc=80：16：4（含0.02 mol/L庚烷磺酸钠）为流动相,检测波长330 nm;对依替米星在生理盐水,5%葡萄糖,10%葡萄糖,复方氯化钠,葡萄糖氯化钠等溶媒中进行了稳定性研究,在室温（17℃）,25℃,35℃情况下,将依替米星与不同的溶媒配伍后,在1 h,2 h,4 h,6 h,8 h分别测定它们的含量及pH值.结果表明依替米星在上述溶媒中的稳定性较好.在pH=2,pH=10,pH=12的条件下对依替米星进行稳定性研究,结果表明,依替米星在pH为2～10时稳定,当pH＞10时依替米星被破坏.     

HPLC法测定注射用头孢哌酮钠舒巴坦钠（2：1）的含量

建立注射用头孢哌酮钠舒巴坦钠（2：1）含量测定的HPLC分析方法。采用ODS色谱柱（150mm×6．0mm,5μm）,流动相为乙腈-水相（23：77）,水相为pH5．0的0．005mol／L氢氧化四丁基铵和0．05mol／LKH2PO4水溶液;检测波长220nm。头孢哌酮和舒巴坦分离度及线性关系良好,回收率分别为99．9％和100．4％,并可同时分离其中的头孢哌酮S异构体、头孢哌酮降解物B及其他相关物质。该方法准确、可靠,适用于注射用头孢哌酮钠舒巴坦钠（2：1）的含量测定,相比于中国药典（2010版）中注射用头孢哌酮钠舒巴坦钠含量测定的流动相有所改进,提高了适用性。     

高效液相色谱法测定贝壳类海洋生物中的多胺含量

利用柱前衍生高效液相色谱法测定了贝壳类海洋生物(蛤蜊、牡蛎、扇贝)中多胺(主要是指亚精胺(SPD)和精胺(SPM))的含量。采取多种提取试剂(如不同浓度的HCl和H2SO4、甲醇、水提醇沉等)考察了样品中多胺的提取效果,另外,确定了最佳提取时间和温度。结果表明:样品中多胺的最佳提取条件为6mol·L-1 HCl溶液,蛤蜊和牡蛎60℃下提取3h,扇贝提取时间4h为好。提取液用丹磺酰氯衍生,甲苯萃取后高效液相色谱分析。色谱条件:流动相为甲醇和水,采用梯度洗脱,柱温40℃,荧光检测。测定结果:亚精胺(SPD)的回归方程为Y=0.172 9+0.261 6 X(R=0.998 8),检出限为0.48pmol;精胺(SPM)的回归方程Y=0.074 0+0.170 4 X(R=0.999 2),检出限为0.54pmol。     

酶反应产物中人参稀有皂苷F2与C-Mc的分离

原人参二醇类皂苷混合物经人参皂苷酶生物转化后可生成F2、C-Mc等7~10种稀有人参皂苷。天然人参中不含人参皂苷C-Mc,且F2的含量极低。在生物转化所得的人参二醇类皂苷酶反应产物中,分离纯化得到稀有人参皂苷F2与C-Mc,并进行HPLC检测。反应后得到粗产品40g,经脱糖脱色和硅胶柱分离后,成功得到稀有人参皂苷F23.49g,纯度为98.2%,得率8.72%;得到C-Mc 0.70g,纯度为82.2%,得率为1.80%。成功分离出了F2和C-Mc制品,建立了初步的分离制备方法。     

五味子木脂素超声循环提取工艺条件的优化

采用超声循环提取的方法从五味子中提取五味子醇甲等木脂素类有效成分,考察溶剂、超声时间、超声功率、液固比和温度对提取工艺的影响．结果表明采用85％的乙醇作为提取溶剂,在单因素实验的基础上通过正交实验得出最佳工艺条件：超声功率500W,超声时间10min,温度30℃,液固比20,五味子木脂素提取率达到80．84％．     

Detection of olive oil adulteration with canola oil from triacylglycerol analysis by reversed-phase high-performance liquid chromatography

The objective of this study was to explore the use of reversed-phase high-performance liquid chromatography (RP-HPLC) as a means to detect adulteration of olive oil with less expensive canola oil. Previously this method has been shown to be useful in the detection of some other added seed oils; however, the detection of adulteration with canola oil might be more difficult due to similarities in fatty acid composition between canola oil and olive oil. Various mixtures of canola oil with olive oils were prepared, and RP-HPLC profiles were obtained. Adulteration of olive oil samples with less than 7.5% (w/w) canola oil could not be detected.     

HPLC analysis of quaternary ammonium surfactants with the evaporative light scattering detector

A normal-phase high-pressure liquid chromatography technique has been elaborated for the separation of quaternary ammonium surfactants. The separation was achieved on a bonded polyphenol silica gel column with gradient elution and evaporative light-scattering (ELS) detection. The proposed method has been applied to the quantitative determination of low levels of monoalkyltrimethylammonium and trialkylmethylammonium chlorides in dialkyldimethylammonium chloride.     

Lipase G-Catalyzed synthesis of monoglycerides in organic solvent and analysis by HPLC

Monoglycerides were synthesized with Lipase G fromPenicillium sp. as biocatalyst. This enzyme successfully catalyzed the esterification of glycerol with oleic acid (18:1 n-9) or eicosapentaenoic acid, EPA (20:5 n-3) in hexane. Esterification at 40°C for 24 hr resulted in 86.3 mol% and 64.3 mol% incorporation of 18:1 n-9 and 20:5 n-3, respectively. Lipase GC fromGeotrichum candidum was not effective in esterifying the fatty acids under the present experimental conditions. Lipase G was able to incorporate 98.5 mol% and 98.1 mol% of 18:1 n-9 onto glycerol in 24 hr or less at 25°C and 37°C, respectively, in the absence of molecular sieve 4A. The product formed was analyzed by high performance liquid chromatography (HPLC) with a combined evaporative light scattering mass detector (ELSD) and ultraviolet detection at 206 nm. The result of this study demonstrates that Lipase G is capable of incorporating long-chain fatty acids of potential health benefit onto glycerol.     

HPLC法研究C.I.Reactive Red 24水解反应动力学

采用反相离子对高效液相色谱法(HPLC)研究了C.I.Reactive Red 24 水解反应动力学.当染料溶液中羟基过量时, 可视为一级反应; -d[A]/dt=k[A].在pH=13时, ln(A0/A)与反应时间t呈线性关系; 95℃时的水解反应速率常数K(0.0599)比70℃时的k(0.0101)高约4倍; pH为13时, 反应速率常数K(5.99×10-2)比8.5时的k(4.8×10-3)高约11.5倍; pH值每升高1, 染料的水解速率相应提高1.5倍.     

反相高效液相色谱法测定苯扎贝特的含量

研究了采用反相高效液相色谱测定苯扎贝特含量的方法 ,以磷酸盐缓冲液 (0 0 1mol/L的磷酸二氢钾用磷酸调节pH至 3 8) 甲醇 (4∶6 )为流动相 ,采用HypersilC18柱 (5 μm ,4 6mm× 15 0mm) ,检测波长为 2 30nm ,苯扎贝特在 0 0 114～0 114mg/mL范围内线性相关 ,回归方程为 :A =1 0 5× 10 4c(mg/mL) +2 70× 10 2 ,r =0 9997,此法简便、快速、结果准确可靠