2-（4-氯苯氨基）甲基苯酚降解的动力学研究

采用高效液相色谱技术,开展了Fenton试剂对2-（4-氯苯氨基）甲基苯酚（CMP）的氧化降解动力学的研究。考察了初始双氧水摩尔浓度、亚铁离子摩尔浓度和温度等因素对CMP降解速率的影响,结果表明,当双氧水摩尔浓度、亚铁离子摩尔浓度增大和温度升高时,CMP的氧化速率明显加快。在30~45℃的温度范围内,其氧化降解符合假一级反应动力学模型,反应的表观活化能Ea为102.90kJ/mol。     

免疫亲和柱法测定小麦中黄曲霉毒素

本文研究了用正相高效液相色谱仪附荧光检测器测定小麦中黄曲霉毒素B1、B2、C1、C2。黄曲霉毒素用甲醇－水（70＋30）提取，提取液经免疫亲和柱富集、净化，于液相色谱仪上测定。本实验采用添加法测定回收率，添加水平为0.11-3.9μg/kg时，其平均回收率为87.9%-102.5%。本方法的最低检测限为0.1μg/kg。     

反相HPLC法测定苦参碱氯化钠注射液中苦参碱含量

建立苦参碱含量测定的R—HPLC方法。采用C18反相柱，流动相为pH3．5磷酸缓冲液(1000ml水 2．0ml三乙胺，然后用磷酸准确调节pH至3．5)-乙腈=96／4，流速1．0ml／min，检测波长210nm，线性范围36．18-84．42μg／ml。     

小麦中脱氧雪腐镰刀菌烯醇的测定及方法研究

利用免疫亲和柱对脱氧雪腐镰刀菌烯醇(DON)的特异吸附性,使用高效液相色谱法对样品进行测定.研究了提取方式、样品粒度、样品溶液稳定性、振荡提取时间等因素对检测结果的影响.当标准曲线在0～2.0 μg/mL之间,线性关系良好,相关系数达到0.999 1.检测结果RSD小于8.0％,不同水平的加标回收率处于92.0％～107.4％之间,通过回收率试验和标准物质试验验证了方法的可靠性和准确性.     

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％．     

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。     

杏酒中有机酸类化合物的RP—HPLC法测定

建立了反相高效液相色谱测定杏酒中有机酸类化合物的方法．以金太阳杏为原料,经液体发酵法精心酿制成的低度杏酒作为检测样品,测定了杏酒中9种有机酸类化合物．采用AgilentC18色谱柱（4．6mm×250mm）分离,流动相2％的甲醇-0．01mol／L（NH4）2HPO4（pH2．8）洗脱,流速1mL／min,检测器波长为210nm,柱温30℃,采用色谱峰保留时间定性,面积外标法定量,并比较了不同杏发酵产品中有机酸的种类和含量,各成分的线性相关系数均大于0．99．方法的回收率大部分都在94％以上,RSD均在3％以下,说明该方法具有快速、分辨率高、重复性好等优点,可用于杏酒中有机酸类化合物的检测．     

HPLC法测定新益肾蠲痹丸中延胡索乙素含量

建立HPLC法测定益肾蠲痹丸中延胡索乙素的含量。采用Kromasil色谱注,流动相为甲醇-乙腈-1%醋酸铵缓冲液（pH=5.0±0.02）（10∶30∶60）,流速1.0ml/min,检测波长283nm。延胡索乙素在0.07776～1.5552ug（r=0.9999）范围内线性关系良好,平均回收率为99.6%。     

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。     

Effects of sample drying and storage,and choice of extraction solvent and analysis method on the yield of birch leaf hydrolyzable tannins

In this study, I investigated the effects of different methods of sample drying and storage, and the choice of extraction solvent and analysis method on the concentrations of 14 individual hydrolyzable tannins (HTs), and insoluble ellagitannins in birch (Betula pubescens) leaves. Freeze- and vacuum-drying of birch leaves were found to provide more reliable results than air- or oven-drying. Storage of leaves at –20C for 3 months before freeze-drying did not cause major changes in tannin content, although levels of 1,2,3,4,6-penta-O-galloylglucose and isostrictinin were altered. Storage of dried leaf material at –20C is preferred because 1 year storage of freeze-dried leaves at 4C and at room temperature decreased the concentration of the pedunculagin derivative, one of the main ellagitannins of birch. Furthermore, storage at room temperature increased the levels of isostrictinin and 2,3-(S)-HHDP-glucose, indicating possible HT catabolism. Of the extraction solvents tested, aqueous acetone was superior to pure acetone, or aqueous or pure methanol. The addition of 0.1% ascorbic acid into 70% acetone significantly increased the yield of ellagitannins, presumably by preventing their oxidation. By comparing the conventional rhodanine assay and the HPLC–ESI-MS assay for quantification of leaf galloylglucoses, the former tends to underestimate total concentrations of galloylglucoses in birch leaf extract. On the basis of the outcomes of all the method and solvent comparisons, their suitability for qualitative and quantitative analysis of plant HTs is discussed, emphasizing that each plant species, with its presumably unique HT composition, is likely to have a unique combination of ideal conditions for tissue preservation and extraction.