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HPLC同时测定血浆中头孢氨苄和甲氧苄啶的浓度 总被引:2,自引:1,他引:2
采用高效液相色谱紫外检测器同时检测血浆中头孢氨苄和甲氧苄啶的浓度。以0.5倍血浆体积,浓度为10%(v/v)的高氯酸为蛋白沉淀剂。色谱条件:Diamonsil C18(250mm×4.6mm,5μm),柱温:30℃,流动相:pH3.0的0.05mol/L的磷酸盐缓冲液∶乙腈∶甲醇(76∶16∶8),流速1.0ml/min,进样量20μl,检测波长240nm。头孢氨苄、甲氧苄啶及内源性物质分离良好。头孢氨苄血药浓度线性范围为0.5~50.0μg/ml,检测限为50ng/ml,高、中、低浓度的相对回收率在97.3%~100.5%之间(n=5),日内RSD≤6.5%(n=5),日间RSD≤8.3%(n=5)。甲氧苄啶血药浓度线性范围为0.25~25.0μg/ml,检测限为25ng/ml,高、中、低浓度的相对回收率在96.5%~99.3%之间(n=5),日内RSD≤6.9%(n=5),日间RSD≤8.6%(n=5)。本法样品处理简单、灵敏、准确,适合于同时测定两者的体内浓度。 相似文献
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目的采用高效液相色谱法(HPLC)测定胆汁中美罗培南的浓度。方法色谱柱:Waters Symmetry C18(4.6mm×150mm,5μm);流动相:乙腈∶0.05mol/L磷酸二氢钾(pH6.5,8∶92);流速1.5ml/min;检测波长300nm;进样量20μl;柱温22.5℃。结果美罗培南的胆药浓度在0.5~500.0μg/ml范围内,浓度与峰面积比的线性关系良好(r=0.9999),胆汁中最低定量限为0.5μg/ml。HPLC方法回收率达96.87%以上(n=15)。日内RSD≤6.22%,日间RSD≤3.69%。结论本方法简单、快速、准确,可用于美罗培南的浓度测定和药动学研究。 相似文献
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目的:测定血浆中头孢布烯的浓度。方法:采用Hypersil-ODS柱,流动相为乙腈:乙酸铵(pH4.98,0.05mol/L)=2:98(V/V),流速为1.00ml/min。结果:标准曲线范围0.3125-20.00μg/ml(r=0.9999),回收率试验大于95%,日内和日间变异(RSD%)小于4%。结论:本法专属性好,操作简便,可用于临床血药浓度的监测。 相似文献
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高效液相色谱法测定人血浆中头孢克肟浓度 总被引:2,自引:0,他引:2
目的:建立HPLC方法测定人血浆中头孢克肟的浓度。方法:取100μl血浆样品,加乙腈混匀离心,上清液进样;用C18分析柱,以0.02mol/L磷酸氢二钾缓冲液(用磷酸调pH=7.00):乙腈=1:1(V/V)为流动相,流速1.0ml/min,柱温25℃,紫外检测波长288nm,用峰面积定量。结果:标准曲线在0.125~4μg/ml范围内线性关系良好(r=0.9999)最低检测浓度为0.125μg/ml;回收率为100.7%~109.3%,日内RSD﹤5%,日间RSD﹤8%。结论:本法简便,准确,精密,快速,进样量少,可满足临床血药浓度测试要求。 相似文献
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用柱切换HPLC法建立了豚鼠血浆和皮下组织液中诺氟沙星银体内主要解离物诺氟沙星的测定方法。预处理柱为μ-BondapakC18,37~50μm,50mm×5mmID;分析柱为YWG-C18,10μm,150mm×5mmID。预处理流动相为0.008mo1/L磷酸缓冲液,流速为3ml/min;分析流动相为甲醇—0.008mol/L磷酸缓冲液—0.05mol/L四丁基溴化铵(25:75:4)。紫外检测波长为280nm。皮下组织液及血浆中的线性范围分别为100~3200ng/ml(r=0.9999)和2~128μg/ml(r=0.9999);最低检测浓度分别为10ng/ml和0.25μg/ml,方法的平均回收率为102%,日内及日间偏差均小于7%。 相似文献
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目的 建立适合于同时测定人血浆中美罗培南与亚胺培南浓度的通用高效液相色谱快速检测方法。方法 采用外标法定量,血浆样品采用适量的乙腈沉淀蛋白,离心后取上层清液加入二氯甲烷萃取,涡旋离心后取上清液,再次离心后进样分析。采用Agilent 1260高效液相色谱仪,色谱柱为Agilent ZORBAX SB-C8(4.6 mm×250 mm, 5μm),流动相为乙腈-0.1 mol·L-1乙酸铵溶液,采用梯度洗脱法,流速为1 mL·min-1,柱温30℃,检测器采用二极管阵列检测器,检测波长为298 nm。结果 美罗培南在1~200μg·mL-1范围内线性良好(r=0.99990),亚胺培南在1~200μg·mL-1范围内线性关系良好(r=0.99957);两种药物的低、中、高浓度(2.0,80.0,200.0μg·mL-1)的日内、日间精密度RSD在0.19%~1.53%范围之内;平均提取回收率在(81.67±6.30)%~(90.83±3.34)%范围之内;方... 相似文献
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目的:建立测定人血浆中法罗培南浓度的高效液相色谱法。方法:血浆样品用30%的高氯酸沉淀,色谱柱为Ultimate C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.02 mol·L~(-1)NaH_2PO_4(pH 3.8)-乙腈=75:25;流速1.0 ml·min~(-1);检测波长为317nm,采用外标法定量。结果:法罗培南在0.02~12μg·ml~(-1)范围内线性良好,日内和日间差均<15%,绝对回收率>70%,结论:本法灵敏度高,操作简便、快速,适用于法罗培南临床药物动力学和生物等效性的研究。 相似文献
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高效液相色谱法测定人血浆中舒乐安定的浓度 总被引:2,自引:1,他引:1
本文应用高效液相色谱法测定人血浆中舒乐安定的浓度。检测波长为240nm,利眠宁为内标,甲醇:磷酸盐缓冲液为移动相。回收率为97.3~108.9%,日内和日间误差(浓度0.60μg/ml)(CV)分别为2.5%和2.9%(n=9)。对临床数十名患者血浓测定,其血浓在0.4~0.87μg/ml,为临床合理用药提供了依据。 相似文献
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目的 探讨以反相高效液相色谱法测定人血清中盐酸二甲双胍的浓度精确性.方法 色谱柱为Kromalsil C18柱,流动相为0.05mol/L磷酸盐缓冲液(内含0.015mol/L的十二烷基磺酸钠,pH4.0)-甲醇(35:60),流速为1.0ml/min,检测波长为233nm.结果 盐酸二甲双胍的线性范围为0.06725~4.304μg/ml,回归方程为Y=184327C+404.13(r=0.9999);日内精密度为3.74%~5.16%,日间精密度为4.26%~5.86%结论本方法操作简便,测定结果准确,重现性好. 相似文献
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目的考察盐酸氨溴索缓释片体外释放度与体内吸收的相关性。方法应用释放度测定法研究盐酸氨溴索缓释片体外释药行为 ,采用HPLC法测定盐酸氨溴索缓释制剂在家犬体内的血药浓度 ,按照Wagner Nelson公式计算药物的吸收分数。 结果 3种自制盐酸氨溴索缓释片与参比制剂生物等效 ,以药物累积吸收百分数 f(t)与相应时刻的体外累积释放百分数F(t)建立的一元线性回归方程 ,参比制剂与 3种自制制剂的体内外相关系数分别为 0 969、0 979、0 970和 0 983。结论盐酸氨溴索缓释片的体外释放度与体内吸收具有显著的相关性。 相似文献
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Kacper A. Wojtal Lutz Wolfram Isabelle Frey-Wagner Silvia Lang Michael Scharl Stephan R. Vavricka Gerhard Rogler 《Toxicology in vitro》2013,27(5):1525-1532
Retinoid treatment is suggested to promote development of inflammatory bowel disease, although preclinical studies are not supportive. We evaluated the effect of retinoids on cytokine response in in vitro-differentiated human dendritic cells (ivDCs) and macrophages (ivMACs) derived from healthy human donors and in cultured human THP-1 cells. Effect on human intestinal epithelial cell integrity was also assessed. Each cell type was incubated (±lipopolysaccharide [LPS]) with all-trans retinoic acid (ATRA), 13-cis-RA (isotretinoin) and 4-oxo-13-cis-RA. Cytokine analysis was performed by array analysis. Cultured human endothelial colorectal adenocarcinoma (Caco-2) cells were incubated with these retinoids and media analyzed for leakage by spectrofluorometric analysis. ATRA consistently and significantly inhibited LPS-induced release of the pro-inflammatory cytokines tumor necrosis factor, interleukin (IL)-6, macrophage inflammatory protein (MIP)-1α and MIP-1β. All retinoids tested stimulated release of the anti-inflammatory cytokines granulocyte–macrophage colony-stimulating factor and IL-10, and also monocyte chemotactic protein-1, vascular endothelial growth factor and eotaxin-1. Incubation with retinoids did not significantly alter the permeability of Caco-2 monolayers. Pre-treatment of each cell type with retinoids promoted an anti-inflammatory cytokine profile with only minimal effect on intestinal epithelial cell permeability; consistent with in vivo studies. 相似文献
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Liu Fang-Yu Sambol Nancy C. Giannini Robert P. Liu Chui Yu 《Pharmaceutical research》1996,13(10):1501-1506
Purpose. A method to establish the in vitro-in vivo relationship of oral extended-release products is proposed.
Methods. The approach utilizes incremental amounts of drug released and absorbed within defined time intervals, to construct a 2 distributed variable for testing in vitro-in vivo similarity.
Results. A case study is used to demonstrate that the similarities between incremental values of in vivo absorbed and in vitro dissolved fractions are distinguishable for different dissolution profiles despite naturally significant linear correlations between cumulative in vivo absorbed and in vitro dissolved fractions (with different dissolution tests) of an oral extended-release product.
Conclusions. The method enables investigators to compare different in vitro dissolution profiles of an oral extended-release product to find an optimized dissolution profile to be the surrogate of the in vivo release process of the product. 相似文献
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Ergosine and its D-isolysergic acid derivative ergosinine were investigated on canine saphenous veins both in vivo and in vitro. Following local i.v. infusion in vivo, about 5 times higher doses of ergosinine were necessary to produce the same venoconstrictor response as induced by ergosine. When administered orally, however, both ergot alkaloids were equi-effective. In vitro methiothepin, a 5-HT receptor blocker with high affinity for 5-HT1 receptors, antagonized venoconstrictor responses to 5-HT and ergosine within the same concentration range, being significantly less potent when tested against norepinephrine. The reverse was true for the α2-selective adrenoceptor blocker yohimbine, which was significantly more potent against norepinephrine and ergosine than against 5-HT, suggesting that ergosine has affinity to both 5-HT1-like receptors and α2-adrenoceptors. Concentration-response curves to norepinephrine were shifted to the right in a parallel fashion when ergosine or ergosinine were present in the organ baths, suggesting competitive antagonism. The blocking potency of ergosinine increased with increasing incubation times in Krebs-Henseleit solution becoming similar to that of ergosine when an incubation time of 2 hr was applied. It is suggested that the pharmacological activity of ergosinine is the consequence of an isomerization into its natural stereoisomer ergosine, which may occur both in vivo and in vitro. 相似文献
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氟罗沙星的体内外试验相关性研究 总被引:4,自引:1,他引:3
本文研究了新型喹诺酮类药物氟罗沙星体外溶出与体内吸收之间的相关性。实验表明,本品口服吸收在血清中达峰时间较快,作用持久,消除半衰期为9.60hr。在人工胃液中溶出速率较快,在血清达峰之前,体内吸收与体外溶出量之间呈现良好的相关性。 相似文献
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B. Sreenivasa Rao A. Seshasayana S. V. Pardha Saradhi N. Ravi Kumar Cheruvu P. S. Narayan K. V. Ramana Murthy 《International journal of pharmaceutics》2001,230(1-2):1-9
The purpose of this study was to investigate the possibility to develop different levels of correlation between in vitro dissolution parameters and in vivo pharmacokinetic parameters for three rifampicin formulations. A level A correlation of in vitro release and in vivo absorption could be obtained for individual plasma level data by means of the Wagner and Nelson method. Linear correlation could be obtained when percent dose released in vitro was plotted vs percent dose absorbed in vivo with correlation coefficients between 0.954, 0.983 and 0.997 for the formulations studied. A second level correlation between mean in vitro dissolution time (MDT) and mean in vivo residence time (MRT) was performed with a correlation coefficient of 0.536, 0.420 and 0.335. Finally, it was also possible to establish a good in vitro–in vivo correlation when the T50%hrs (time taken to release 50% of rifampicin) in vitro and Cmax, Tmax or AUC in vivo were compared. 相似文献