HPLC-UV法测定箭羽糖康片中芒果苷的含量

目的建立箭羽糖康片质量控制方法。方法采用HPLC-UV法测定箭羽糖康片中芒果苷的含量,流动相为乙腈-水（12∶88）,用0.85%的磷酸调pH至2.85,流速0.8ml/min,检测波长258nm。柱温30℃。结果芒果苷在3.9-390μg/ml范围内呈现良好的线性关系（r=0.9999）。样品平均回收率为97.718%,RSD为0.92%。结论建立HPLC-UV法测定箭羽糖康片中的芒果苷含量,方法简便准确,灵敏度高,能有效地控制制剂质量。     

HPLC同时检测丹参提取物中5种水溶性和脂溶性成分含量

目的:建立丹参提取物中丹酚酸A、丹酚酸B、紫草酸、丹参素及丹参酮ⅡA反相HPLC同步测定新方法.方法:选用Kromasil 100-5 C18(4.6 mm × 250 mm,5μm)色谱柱,以乙腈-水(含0.1％甲酸)为流动相梯度洗脱,流速1 mL· min-1,检测波长285 nm.结果:丹酚酸A、丹酚酸B、紫草酸、丹参素及丹参酮ⅡA分别在进样量范围内与峰面积线性关系良好,r＞0.999 5,仪器精密度和稳定性RSD均＜2％,成分的回收率在97％ ～ 103％(n=3).测定了其5批丹参提取物含量.结论:该方法快速、准确、重复性好,可同时定量丹参的5种水溶性及脂溶性成分.     

单剂量静脉滴注兰索拉唑在中国健康人体的药代动力学

目的 研究中国健康志愿者单次静脉滴注兰索拉唑(抑胃酸药)的药代动力学特点.方法 12名健康志愿者,先后单次静滴3个剂量(15,30,60 mg)兰索拉唑;用高效液相色谱-紫外检测法测定给药后不同时间点的血药浓度,用3P97软件计算药代动力学参数.结果 血药浓度-时间曲线符合二房室模型,健康受试者单次静滴3个剂量(15,30,60 mg)兰索拉唑后主要的药代动力学参数:C_(max)分别为(1105.65±506.24),(2171.33±799.02),(4070.53±643.04)μg·L~(-1);t_(1/2)分别为(1.63±0.86),(2.30±2.01),(1.90±1.19)h;AUC_(0-12)分别为(991.16±814.49),(3495.87±1770.92),(8351.14±2599.90)μg·h·L~(-1).结论 兰索拉唑的体内过程在男女性别间无显著差异,剂量在15～60 mg内较安全.     

Design of packed-fiber solid-phase extraction device for analysis of the drug and its metabolite in plasma

A mini-column packed with 1 mg electrospun polystyrene nanofibers (about 200∼400 nm in diameter) was designed for simple, fast extraction of drugs, diazepam and its major metabolite, N-desmethyldiazepam for the analysis of them in human and dog plasma. Ttrezodone was selected as internal standard. The drugs adsorbed on the solid phase could be desorpted with 50 μl of the methanol and then monitored by liquid chromatography coupled to an ultraviolet detector. Parameters influencing the extraction efficiency such as fiber packing amount, eluted solvent, and pH of the sample were decided. The time for the pretreatment of 0.5 ml plasma sample was less than 10 min. The detection limits of diazepam and N-desmethyldiazepam in plasma could be as low as 1 μg/L. The intra- and inter-day precision, calculated from quality control (QC) samples, was less than 9.1%. The method was evaluated by its application in determination of dog plasma samples from three beagles after a single dose oral of diazepam. The technique was validated by comparison with conventional plasma analysis. It was observed that the mini-column offers improved limits of detection and reduced sample preparation time as compared to conventional method. For its simplicity and sensitivity, the method may be used in therapeutic drug monitoring and pharmacology study.     

高效液相色谱法测定人全血中瑞芬太尼浓度

目的:建立测定人血中瑞芬太尼的高效液相色谱-紫外检测方法,为临床监测血药浓度提供方法学.方法:采用液-液萃取法,用1-氯丁烷提取全血中的瑞芬太尼,选用GI97559(瑞芬太尼乙基类似物)为内标定量.色谱柱为Zorbax SB-CN(4.6 mm×250 mm,5 μm),流动相为乙腈-甲醇-磷酸二氢钠缓冲液(1∶2∶0.43),柱温30℃,流速1.5mL*min-1,紫外210 nm检测,按内标法定量.结果:标准曲线在3～200 μg*L-1范围内,浓度与峰面积比有良好的线性关系(r=0.9966).最低检测浓度为2μg*L-1.提取回收率77.34%～87.72%.方法回收率97.13%～100.99%,日内RSD小于5.3%,日间RSD小于6.3%.结论:本方法快速、准确、灵敏,可用于瑞芬太尼的临床药动学研究.     

控释和缓释地尔硫卓胶囊在健康人体的生物等效性

目的研究地尔硫卓缓释和控释制剂(降压药)在健康人体的生物等效性。方法采用随机交叉给药方法,18名健康受试者单次和多次口服缓释或控释地尔硫卓胶囊。用高效液相色谱-紫外检测法测定血浆中的地尔硫卓浓度,用Winnolin软件计算药代动力学参数。结果控释和缓释地尔硫卓胶囊主要药代动力学参数,单次:tmax分别为(14.1±3.9)和(8.4±4.1)h,Cmax分别为(73±37)和(94±44)ng·mL-1,AUC0-36分别为(1348±590)和(1571±679)ng·h·mL-1,t1/2分别为(7.9±2.9)和(8.0±3.5)h。多次:tmax分别为(8.1±5.0)和(4.83±2.73)h,Cmax分别为(145±41)和(170±58)ng·mL-1,AUCss分别为(2232±642)和(2419±658)ng·h·mL-1,波动度DF分别为(103±32)%和(123±32)%。结论多次给药后,控释和缓释地尔硫卓具有生物等效性。     

大鼠体内恩丹西酮与氯丙嗪的药动学相互作用研究

 目的建立同时测定大鼠血浆中恩丹西酮、氯丙嗪的HPLC-UV分析方法,探索恩丹西酮与氯丙嗪在大鼠体内药动学的相互作用,并进行高蛋白食物对2种药物药动学影响的研究。方法以替米沙坦为内标,乙酸乙酯提取,HPLC-UV分离、分析。色谱系统:C₈柱(4.6mm×250mm,5μm),甲醇-水(70:30)为流动相,流速1.0mL·min^-1,柱温30℃。以大鼠为研究对象,分别在禁食和服用高蛋白食物状态下给以恩丹西酮、氯丙嗪或联合使用2种药物。用建立的血药浓度测定方法测定,计算其药动学参数并进行t检验。结果联合用药后,恩丹西酮的ρ_max,t_1/2,MRT,AUC_0→t,AUC_0→∞与单独用药时相比显著性增加。氯丙嗪单独用药和联合用药时的ρ_max,t_1/2,MRT,AUC_0→t,AUC_0→∞无显著性差异。高蛋白食物能使恩丹西酮的ρ_max,AUC_0→t,AUC_0→∞明显增加,使氯丙嗪的t_max延长,ρ_max,AUC_0→t,AUC_0→∞降低。结论恩丹西酮和氯丙嗪联合使用时,恩丹西酮的药动学过程会受到显著性影响;食用高蛋白食物后,恩丹西酮和氯丙嗪的药动学参数均会发生明显的改变,应在临床使用中注意这些问题,适当调整药物剂量。     

Quantification of microcystins in natural waters by HPLC-UV after a pre-concentration step: validation of the analytical performances and study of the interferences

A method for the determination of microcystins concentrations (MC-LR, MC-RR, MC-YR) in natural water samples was optimized using High Performance Liquid Chromatography with UV/PDA detection after Solid Phase Extraction. Solid Phase Extraction is needed to clean natural sample and concentrate pollutant. The method was validated by evaluation of specificity and repeatability. Average recoveries in ultra-pure grade water were better than 95% with Relative Standard Deviation values lower than 4%. Matrix interferences, as pH, conductivity and organic matter content, were tested. pH must be fixed between 6 and 8 to avoid under-estimation or over-estimation and conductivity did not interfere with the analytical method. Organic Matter content negatively impacted microcystins quantification unlike organic matter characteristics. It over-estimated the concenration by an average of 19%. Then, the developed method was applied to study the occurrence of microcystins in Pigeard pond (France). These results constitute the first report on the concentration levels and seasonal variations of microcystins in this resource water.     

高效液相色谱-紫外/质谱评价海洋天然产物体外抑制环氧合酶2活性方法研究

目的 建立基于高效液相色谱-紫外和高效液相色谱-多级离子阱质谱分析的海洋天然产物体外抑制COX-2酶的活性评价方法。方法 采用Agilent Poroshall 120 C18 色谱柱,以乙腈-0.05%磷酸水溶液为高效液相色谱流动相,二元等度洗脱,流速为0.4 mL?min-1,检测波长为210 nm,进样量10 μL;质谱条件下,流动相改为乙腈-0.05%乙酸水溶液,进样量为1 μL,选用ESI离子源,负离子电离模式,喷雾气压35 psi,干燥气（N2）流速12 L?min-1,干燥气温度350 ℃。结果 建立的高效液相色谱-紫外和高效液相色谱-多级离子阱质谱法精密度和稳定性良好,对比两者测定酶底物花生四烯酸的适用性显示,基于HPLC-UV的评价方法适用极性较大的天然产物粗提物;HPLC-IT-MS/MS法则因其抗干扰能力强适用于复杂体系中极性较弱的活性物质的检测。以建立的HPLC-UV和HPLC-IT-MS/MS方法对海洋天然产物的COX-2酶抑制活性进行评价,天然产物粗提物中黄海葵Anthopleura lanthogrammica berkly乙醇粗提物和弯孢菌Curvularia lunata strain L2744发酵液粗提物对COX-2酶抑制作用较为明显,抑制率分别为70.1%和25.48%。结论 建立的评价方法具有适用性强、结果可靠等优点,有望为天然产物粗提物中COX-2酶抑制剂体外筛选的提供技术参考。     

奥氮平血药浓度的测定及其人体药代动力学

目的 建立测定人血浆中奥氮平浓度的HPLC－UV方法，研究健康受试者口服奥氮平片后的药代动力学。方法 以阿米替林为内标，血浆样品加维生素C抗氧化，经碱化后用乙醚－环已烷进行萃取。以0.01mol/L磷酸铵（pH4.0)－甲醇－乙腈（55：22.5：22.5）为流动相，采用Hypersil silica柱进行分离，紫外270nm处进行测定。结果 方法的专属性较好；低、中、高浓度（1.19,9.50,38.00ng/ml）的平均提取回收率分别为81.97,93.47和96.72。该法在1.19-38.00ng/ml浓度范围内呈线性关系，最低检测浓度为1.19ng/ml，日内、日间RSD分别小于9％和12％。用此法测定了20名健康受试者单剂量po奥氮平片后的血药浓度经时变化过程。结论 该法灵敏度高，重现性好，操作简便，适用于临床药代动力学研究和血药浓度监测。