本文以肉桂酸甲酯、水合肼及水杨醛为原料,设计合成了一种"turn-on"型离子选择性荧光探针,采用NMR、IR及HRMS对其结构进行了表征,结果表明该探针为N'-[(2-羟苯基)亚甲基]-3-{2-[(2-羟苯基)亚甲基]肼-1-基}-3-苯丙酰肼(ZL).基于其存在的酰基和邻羟苯基亚甲基胺结构,研究了其对不同金属离子的识别作用,结果Zn2+、Mg2+和Cd2+对探针ZL荧光表现出"turn-on"效应,其荧光分别增强了47、21、24倍,而其他金属离子对其荧光光谱及强度无影响,化合物ZL表现出对Zn2+、Mg2+和Cd2+的高选择性识别和高灵敏检测,其检出限分别为5.5nmol·L-1、8.4nmol·L-1、9.9 nmol·L-1.通过Job's plot实验表明ZL与Zn2+、Mg2+和Cd2+的结合比为1:1,结合核磁滴定及Gaussian计算结果,可推测Zn2+和Cd2+与ZL的酚羟基结合;Mg2+与ZL中的酚羟基、羰基氧及席夫碱的氮原子结合.本文设计的荧光探针ZL可望实现对Zn2+、Mg2+、Cd2+的快速高灵敏检测,在生物以及环境样本的监测中具有较好的应用前景.

目的 研究以低酯果胶为材料的载姜黄素结肠定位栓塞型胶囊的体外释药情况,评价其结肠定位的释药特性.方法 将非渗透性胶囊体、姜黄素自微乳微丸、栓塞片以及肠溶性囊帽组装成栓塞型胶囊,考察栓塞片处方中各因素对释药时滞的影响,评价其在模拟结肠环境中的体外释药行为.结果 当羟丙甲纤维素的型号为K4M、低酯果胶∶羟丙甲纤维素=9.5∶0.5和片重为100 mg时,可达到结肠定位需要的释药时滞.具有相同处方栓塞片的胶囊在5％大鼠盲肠内容物溶液和0.5％果胶酶溶液中的释药时滞均缩短,说明其具有酶降解性.结论 载姜黄素低酯果胶栓塞型胶囊具有酶降解-时滞型结肠定位释药特性.

The experiment conditions for ultrasonic extraction of total saponin from Codonopsis pilosula were discussed.The orthogonal test design was adopted to optimize the factors of the extraction process of total saponin in Codonopsis pilosula,and the colorimetric method was used to determine the contents of total saponin.The new method was compared with the traditional extraction methods.The optimum ultrasonic extraction conditions were as follows;adding methanol,the ratio of solid to liquid 1:20g/mL and ultrasonic extracting three times for 30min each time.The method is simple with stable conditions,and improved the utilization of medical material,that can be used to extract total saponin from Codonopsis pilosula.

OBJECTIVE: To establish the method for the determination of 4 residual organic solvents in finasteride raw materials, i.e. methanol, acetone, chloroform and methylbenzene. METHODS: Headspace gas chromatography was adopted. The residual organic solvents were separated on Phenomenex ZB-624 capillary column using dimethyl sulfoxide as solvent by temperature programming. FID was used as detector with a temperature of 250 ℃. The inlet temperature was 200 ℃. N2 was used as carrier gas with split ratio of 5 ∶ 1. With headspace sampling, equilibrium temperature was 80 ℃ and equilibrium time was 45 min. RESULTS: The linear ranges of methanol, acetone, chloroform and methylbenzene were 12.0-1 200, 10.0-1 000, 1.20-120 and 1.78-178 μg/ml (r=0.999 6～0.999 8), respectively. Recovery rates were 94.7%-97.5% (RSD2.1%); the detection limits were in the rang of 0.021 6 to 10.93 μg/ml. Residual amount of 4 organic solvents in 5 batches of samples were in line with the requirements of Chinese Pharmacopeia (2010 edition). CONCLUSIONS: The method is sensitive and reproducible. It can be applied for the determination of the residual organic solvents in finasteride raw materials.

Objective:To establish an HPLC method for the determination of vinorelbine tartrate in and out of cells.Methods:The vinorelbine tartrate was frozen and defrosted time and again.Then the sample was extracted with methanol and determined through Lichrospher C18(4.6 mm×250 mm,5 μm)column in a mobile phase of 50 mmol/ml potassium phosphate buffer(pH 3.5) and acetonitrile(70:30 v/v) with the flow rate of 1.0 ml/min at 30℃.The detection wavelength was 269 nm.Result: It was accurate and sensitive with a linear range from 0.5 μg/ml to 25 μg/ml for Vinorelbine Tartrate.The mean extraction recovery of extracellular fluid obtained was 84.6%,and the absolute recovery was 100.3%.Intra-and inter-day periods expressed as percent R.S.D.were≤4.84%.For intracellular fluid,the mean extraction recovery was 88.2% and the absolute recovery was 98.3%.Intra-and inter-day periods expressed as percent R S D were≤4.69%.The lowest limit of quantification was 0.5 μg/ml.Conclusion:This method is simple,rapid,accurate and selective for the determination of VCR.

Objective To establish a HPLC method for detecting the content of Mycophenolate Mofetil Capsules.Methods The Zorbax Eclipse XDB-C8 column (150 mm×4.6 mm,5μm) was used,and the mobile phase was triethylamine phosphate buffer solution (pH=5.3)-acetonitrile (65 ∶ 35),the column temperature was 45 ℃ with the flow rate of 1.5 mL/min and the detection wavelength of 250 nm.Results The linear range of mycophenolate mofetil was 0.062 1-0.621 1 mg/mL(r=0.999 8).The average recovery rate was 100.08% ,RSD=0.51% (n=9).Conclusion The method is accurate,simple,rapid and suitable for the quality control of Mycophenolate Mofetil Capsules.