20%虫酰肼悬浮剂的反相高效液相色谱测定

叙述了采用反相高效液相色谱外标法,以甲醇-水作为流动相,用C18柱和紫外检测器(240nm),测定了20%虫酰肼悬浮剂的含量.结果表明:方法的标准偏差为:0.071;变异系数为:0.35%;平均回收率为:99.56%.线性相关系数为:0.9993.     

柱前衍生反相高效液相色谱法快速测定3,5-二氯苯甲酰氯

以无水甲醇作柱前衍生试剂，建立了反相高效液相色谱法间接测定3，5-二氯苯甲酰氯的新方法。实验结果表明，在流动相：甲醇-水（85：15），流速：1．0mL／min，检测波长：288nm的条件下，定量校正曲线具有良好的线性关系，相关系数（r）为0．9999。方法用于样品中标题物质的测定，RSD=0．19％（n=6），加标回收率为99．9％-105％。     

大鼠灌胃中国蜂胶醇提物后血浆中5种酚酸类成分的HPLC测定及其药代动力学

对大鼠灌胃蜂胶乙醇提取物（EEP）后,血浆中5种酚酸类成分的药代动力学特性进行研究.用HPLC-UV法测定血浆中咖啡酸、香豆酸、阿魏酸、异阿魏酸和3,4-二甲氧基肉桂酸的浓度.应用WinNonlin非典型房室模型计算软件计算相应的药代动力学参数.血浆中内源性物质和内标对酚酸类成分测定无干扰,回收率、准确度及日内、日间精密度均符合生物样品测定要求.结果表明,该方法简便、快速、重复性好,适用于咖啡酸等5种蜂胶中酚酸类成分的大鼠血药质量浓度测定及体内药动学研究.     

RP-HPLC测定人参茎叶总皂苷及不同部位浸膏中Rb_3的质量分数

采用反相高效液相色谱法(RP-HPLC)测定人参不同部位浸膏及人参茎叶总皂苷中人参皂苷Rb3的质量分数。色谱柱,Nava-Pak-C18(3.9mm×150mm,4μm);流动相,V(甲醇)∶V(水)∶V(磷酸)=65∶35∶1;检测波长,203nm;体积流量,1.0mL/min;采用外标法测定人参皂苷Rb3质量分数。结果表明,人参皂苷Rb3在0.8～20.0μg呈良好的线性关系(R=0.999 9),平均加样回收率为100.3%。     

辛.溴氟乳油的反相高效液相色谱分析

采用ＲＰ－ＨＰＬＣ技术，以双内标法一次进样同时测定辛硫磷和溴氟菊酯混配乳油中的两种有效成分含量。在选定的色谱条件下，两种有效成分与两个内标物之间以及与乳油中其他组分之间可实现完全分离。该法准确快速，精度度好。辛硫磷的回收率为９９．２９－１００．７％，溴氟菊酯的回收率为９９．３４％－１００．２％，辛硫磷ＲＳＤ％＝０．２６％，溴氟菊酯ＲＳＤ％＝２．５１％。     

反相高效液相色谱法测定肾康口服液中黄柏的小檗碱含量

建立反相高效液相色谱法测定肾康口服液中黄柏的小檗碱含量。采用反相高效液相色谱法,Novapak C18柱(3.9×150mm,5μm)流动相为甲醇一乙腈(0.05mol·L-1)-磷酸二氢钠溶液(20∶3S∶45),流速为1.0mL·min-1,检测波长为346nm。小檗碱的回归方程为C=1.2616+1821X10-6A,r=0.9992,在4.00~20.00μg·mL-1范围内呈线性关系。平均回收率和RSD分别为101.32%和1.18%(n=5)。方法操作简便,测定结果准确可靠,可用于测定肾康口服液中黄柏的小檗碱含量。     

柱前衍生化高效液相色谱法分离胺类对映异构体

以2,3,4,6-四乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)为手性衍生化试剂,采用反相高效液相色谱法分离8种氨基酸和两种手性药物。样品与手性试剂柱前衍生后,在C18柱上,波长为254nm,甲醇-1%三乙胺/醋酸为流动相的反相条件下,能快速达到基线分离,考察衍生化时间和试剂用量、流动相pH值和流速对分离的影响。并把它用于测定1,2-二胺基环己烷的对映异构体过量(ee)值,得到了满意的结果,方法简易、快速。对某些不对称合成中胺类化合物的ee值测定及日常生活中氨基酸异构体的分析具有一定的应用价值。     

A Validated Stability Indicating High Performance Reverse Phase Liquid Chromatographic Method for the Determination of Cilostazol in Bulk Drug Substance

ABSTRACT

A simple, rapid and accurate reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantitative determination of cilostazol. The developed method is also applicable for the related substance determination in bulk drugs. The chromatographic separation was achieved on reversed-phase C-18 column. Eluents were monitored on photo-diode array detector at a wavelength of 210 nm using a mixture (50:50) of water and acetonitrile. Solution concentrations were quantified by external calibration. In the developed HPLC method, resolution between cilostazol and its potential impurities, namely Imp-A, Imp-B, and Imp-C were found greater than two. The drug was subjected to stress condition of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in alkaline medium stress condition. The developed RP-HPLC method was validated with respect to linearity, accuracy, precision, stability of analytical solutions, and robustness.     

无标样RP-HPLC测定α-吡咯烷酮乙酸甲酯

α-吡咯烷酮乙酸甲酯是一种医药中间体,建立了一种RP-HPLC方法,可以在没有α-吡咯烷酮乙酸甲酯标准对照品的情况下,测定合成样品中α-吡咯烷酮乙酸甲酯的含量,当α-吡咯烷酮乙酸甲酯含量为91%~96%时,SD为0.63%~0.82%,RSD为0.66%~0.89%,与化学分析法对比,结果令人满意。     

PG-2, a Potent AMP against Pathogenic Microbial Strains,from Potato (Solanum tuberosum L cv. Gogu Valley) Tubers Not Cytotoxic against Human Cells

In an earlier study, we isolated potamin-1 (PT-1), a 5.6-kDa trypsin-chymotrypsin protease inhibitor, from the tubers of a potato strain (Solanum tuberosum L cv. Gogu Valley). We established that PT-1 strongly inhibits pathogenic microbial strains, but not human bacterial strains, and that its sequence shows 62% homology with a serine protease inhibitor. In the present study, we isolated an antifungal and antibacterial peptide with no cytotoxicity from tubers of the same potato strain. The peptide (peptide-G2, PG-2) was isolated using salt-extraction, ultrafiltration and reverse-phase high performance liquid chromatography (RP-HPLC). Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF/MS) showed the protein to have a molecular mass of 3228.5 Da, while automated Edman degradation showed the N-terminal sequence of PG-2 to be LVKDNPLDISPKQVQALCTDLVIRCMCCC-. PG-2 exhibited antimicrobial activity against Candida albicans, a human pathogenic yeast strain, and Clavibacter michiganensis subsp. michiganensis, a plant late blight strain. PG-2 also showed antibacterial activity against Staphylococcus aureus, but did not lyse human red blood cells and was thermostable. Overall, these results suggest PG-2 may be a good candidate to serve as a natural antimicrobial agent, agricultural pesticide and/or food additive.