共查询到20条相似文献,搜索用时 103 毫秒
1.
目的:建立高效液相色谱法,测定乙胺吡嗪利福异烟片中利福平、异烟肼、吡嗪酰胺和盐酸乙胺丁醇含量。方法:利福平、异烟肼和吡嗪酰胺用C18色谱柱(150mm×4.6mm,5μm),以-0.01M磷酸二氢钾溶液-乙腈为流动相进行梯度洗脱,流速1.0ml·min^-1,检测波长254nm。盐酸乙胺丁醇选用C18色谱柱(150mm×4.6mm,5μm),四氢呋喃-0.4%庚烷磺酸钠(含有0.016%硫酸铜,用磷酸调pH至4.5)(25:75)为流动相,流速1.0ml·min^-1,检测波长258nm。结果:利福平、异烟肼、吡嗪酰胺及盐酸乙胺丁醇线性范围分别为16~160μg·ml^-1(r=0.9999),16—160μg·ml^-1(r=0.9999),53—532μg·ml^-1(r=0.9998),80~320μg·ml^-1(r=0.9998),平均回收率为99.3%~99.5%。结论:方法简便,准确,可用于乙胺吡嗪利福异烟片中各组分的质量控制。 相似文献
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HPLC法同时测定复方川芎胶囊中阿魏酸和川芎嗪含量 总被引:1,自引:0,他引:1
目的:建立用高效液相色谱同时测定复方川芎胶囊中阿魏酸和川芎嗪含量的方法。方法:用Inertsil ODS2 C18柱(150mm×4.6mm,5μm),流动相:甲醇-0.5%冰醋酸溶液(25:75),检测波长:280nm,流速:1.0m1·min^-1。结果:阿魏酸和川芎嗪的线性范围分别为4.4-44μg·ml^-1(r=0.9999)和2.0—20.2μg·ml^-1(r=0.9998),平均回收率分别为100.6%(RSD2.1%)和100.9%(RSD 2.2%)(n=6)。结论:该法简单、快速、重复性好,可用于样品的含量测定及质量控制。 相似文献
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HPLC法同时测定三七中7种皂苷含量 总被引:4,自引:0,他引:4
目的:建立HPLC法同时测定三七中7种皂苷含量的方法。方法:Hypersil BDS C18色谱柱(250mm×4.6mm,5μm);流动相:乙腈(A)-水(B)二元梯度洗脱;流速:1.0ml·min^-1;检测波长203nm;柱温:室温。结果:三七皂苷R1,人参皂苷Rb1,Rb2,Rc,Rd,Rg1,Re的线性范围分别为5.6~140μg·ml^-1(r=0.9992)5.8~144μg·ml^-1(r=0.9991)、5.9-148μg·ml^-1(r=0.9997)、6.1~152μg·ml^-1(r=0.9992)、5.8~144μg·ml^-1(r=0.9992)、5.8~146μg·ml^-1(r=0.9990)、5.8~144μg·ml^-1(,=0.9994);回收率98.5%~100.1%。结论:HPLC法可同时并且简单快速分离三七中7种皂苷。 相似文献
4.
目的:采用高效液相色谱法测定祖卡木胶囊中大黄素和大黄酚的含量。方法:采用Waters Symmetry C18(150mm×4.6mm,5μm)色谱柱,流动相:甲醇-0.1%磷酸溶液(80:20);检测波长:254mm;流速1.0ml·min^-1;柱温35℃。结果:大黄素在0.8—6.6μg·ml^-1(r=0.9999,n=5)范围内,有良好的线性关系,平均回收率为98.8%(n=9),RSD为1.7%。大黄酚在2.0—10.2μg·ml^-1(r=0.9999,n=5)范围内,有良好的线性关系,平均回收率为101.3%(n=9),RSD为1.6%。结论:方法具有操作简单、准确的优点,能有效控制祖卡木胶囊的质量。 相似文献
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目的:建立消炎利胆片中穿心莲内酯和脱水穿心莲内酯的含量测定方法。方法:以XTerra RPC18色谱柱为分离柱,以甲醇-水(45:55)为流动相,采用HPLC法测定。结果:本品中穿心莲内酯含量测定线性范围为16—160μg·ml^-1(r=0.9999),平均回收率为98.87%(RSD=1.90%,n=6);脱水穿心莲内酯含量测定线性范围为32~320μg·ml^-1(r=0.9999),平均回收率为99.54%(RSD=1.93%,n=6)。结论:此法操作简单、结果准确,可用于消炎利胆片的质量控制。 相似文献
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目的:建立反相高效液相色谱法同时测定茶碱麻黄碱胶囊中茶碱和盐酸麻黄碱含量的方法。方法:色谱柱为C18柱(150mm×4.6mm,5μm),流动相为甲醇-0.06mol·L^-1磷酸二氢钾溶液(用磷酸调节pH至2.5)(13:87),流速为0.8ml·min^-1,检测波长为210nm,柱温35℃。结果:茶碱和盐酸麻黄碱浓度分别在18.4—183.8μg·ml^-1(r=0.9998)和4.1-40.8μg·ml^-1(r=0.9993)范围内与峰面积呈良好的线性关系,平均回收率分别为98.9%(RSD=1.1%)和97.6%(RSD=1.2%)。结论:方法简便、准确、重复性好,可用于该制剂的质量控制。 相似文献
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目的:建立以反相高效液相色谱法测定口腔溃疡涂剂中甲硝唑和盐酸丁卡因含量的方法。方法:色谱柱为Thermo ODS hypersilC18(50mm×4.6mm,5μm);流动相为甲醇-水-乙腈-三乙胺(35:50:15:0.7)(用冰醋酸调pH=6.8);流速1.0ml·min^-1;检测波长为310nm;柱温20℃。结果:甲硝唑和盐酸丁卡因分别在20.2~161.6μg·ml^-1(r=0.9994)和6.68~53.44μg·ml^-1(r=0.9993)范围内线性关系良好,平均回收率分别为99.89%(RSD0.62%)和99.84%(RSD0.67%)。结论:本法简便、快速、重复性好,可用于口腔溃疡涂剂的质量控制。 相似文献
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RP-HPLC测定心脑康胶囊中阿魏酸和葛根素的含量 总被引:3,自引:0,他引:3
目的:建立心脑康胶囊中阿魏酸和葛根素的RP—HPLC含量测定方法。方法:色谱柱为DIKMA-C18(250mm×4.6mm,5μm),流动相为甲醇-1%的冰醋酸(30:70),流速为1.0ml·min^-1,检测波长为254nm,柱温为室温。结果:阿魏酸和葛根素的的线性范围分别为11.2-67.2μg·ml^-1(r=0.9994),9.0~54μg·ml^-1(r=0.9992),平均回收率分别为98.5%、98.2%,RSD为0.5%、0.8%(n=5)。结论:方法简便,结果准确,可作为心脑康胶囊的质量控制方法。 相似文献
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目的:研究青霉素V钾咀嚼片在健康人体的药物动力学及生物等效性。方法:19名健康志愿者随机双交叉、单剂量口服受试制剂和参比制剂0.472g,用液相色谱-串联质谱法(LC—MS/MS)测定人血浆中青霉素V的浓度,利用DAS2.0药物动力学软件计算有关药物动力学参数、相对生物利用度,并评价2种制剂的生物等效性。结果:受试制剂和参比制剂的tmax分别为(0.54±0.09)h和(0.53±0.13)h;Cmax分别为(10.64±3.84)μg·ml^-1和(10.87±4.43)μg·ml^-1;t1/2分别为(0.74±0.20)h和(0.75±0.10)h。AUC0-6h分别为(11.92±4.04)μg·ml^-1·h和(12.34±4.17)μg·ml^-1·h;AUC0-∞分别为(12.00±4.04)和(12.43±4.17)μg·ml^-1·h。青霉素V钾咀嚼片的相对生物利用度为(97.9±12.8)%。结论:两种制剂具有生物等效性。 相似文献
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目的:建立HPLC法测定雅静胶囊中厄贝沙坦和氢氯噻嗪的含量。方法:色谱柱:Dianmonsil TMC18柱(250mm×4.6mm,5μm);流动相:乙腈-0.08mol·L^-1磷酸溶液(用三乙胺调至pH5.0)(40:60);流速:1ml·min^-1;紫外检测波长:225nm;进样量:20μl;柱温:25℃。结果:厄贝沙坦和氢氯噻嗪分别在15~135μg·ml^-1(r=0.9999)和1.2~10.8μg·ml^-1(r=0.9999)浓度范围内线性关系良好,平均回收率分别为100.0%和100.5%。结论:本方法操作简便、快捷,重复性好,灵敏度高,结果准确可靠,适用于雅静胶囊的质量控制。 相似文献
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A high-performance liquid chromatographic (HPLC) assay was developed for pyrimethamine in plasma, red blood cells (RBCs), and buffer for the purpose of studying its plasma protein binding and RBC partitioning. Pyrimethamine (1000 ng/ml) was 94% bound to plasma proteins on average, depending on the pH of plasma. A comparison of the lower and upper range of plasma concentrations that would be achieved after a malaria prophylaxis dosing regimen (25 mg/week) showed that the fraction unbound was significantly lower at 120 ng/ml than at the upper plasma concentration of 360 ng/ml, 3.5 vs 4.9%, respectively. Nonlinear regression of the effect of albumin concentration (g/L) on plasma binding yielded the equation: fraction unbound = 1/[(0.421 * albumin concentration) + 1] (R
2 = 0.99). There was no binding to normal levels of alpha1-acid glycoprotein (AAG). The mean ratio of the concentration of pyrimethamine in RBCs to that in plasma (RBC:plasma ratio) was 0.42, while the mean RBC:buffer ratio was 5.2. Binding to hemolysate did not account for all of the RBC uptake, suggesting that binding to or partitioning into RBC membranes may be important. Because pyrimethamine binding depends on both albumin concentration and pyrimethamine concentration in the plasma, these studies predict greater free fractions of pyrimethamine associated with the higher doses given for toxoplasmosis (75 mg/day) and with the hypoalbuminemia associated with AIDS and malaria. 相似文献
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Muhammad Zaman Khan Assir Hafiz Ijaz Ahmad Javed Akram Noshin Wasim Yusuf Umair Kamran 《Basic & clinical pharmacology & toxicology》2014,115(3):291-296
We investigated an outbreak of darkening of skin, bleeding from multiple sites, leucopenia and thrombocytopenia in ischaemic heart disease patients. Case patients were defined as patients who had received medicines from the pharmacy of Punjab Institute of Cardiology between 1 December 2011 and 12 January 2012 and who developed any one of the following: darkening of skin, bleeding from any site, thrombocytopenia and leucopenia. Clinical and drug‐related data were abstracted. All 664 case patients had received iso‐sorbide‐mono‐nitrate contaminated with about 50 mg of pyrimethamine, and 151 (23%) died. The median age of 117 patients admitted at Jinnah Hospital Lahore was 57 years (range, 37–100) and 92 (79%) were male. The median time from intake of medicine to presentation was 37 days (range 13–72). Symptoms and signs included bleeding (in 95% of the patients), skin hyperpigmentation (in 61%), diarrhoea (in 53%) and abdominal pain (in 48%). At presentation, the median white cell count was 2.3 × 109/L (range, 0.1 × 109–16.0 × 109), the median hemoglobin concentration was 109 g/L (range 58–169) and the median platelet count was 18 × 109/L (range, 0 × 109–318 × 109). Bone marrow examination revealed trileneage dysplasia and severe megaloblastosis. The predictors of mortality included presentation prior to 15 January 2012, age more than 57 years, hypotension and leukocyte count less than 1.5 × 109/L. None of the patients who died received Calcium folinate because all deaths occurred prior to contaminant identification. We describe an outbreak of pyrimethamine toxicity in ischaemic heart disease patients receiving medicines from a single pharmacy due to accidental contamination of iso‐sorbide mono‐nitrate tablets at industrial level. Late recognition of illness resulted in high mortality. 相似文献
14.
M. D. Coleman G. W. Mihaly G. Edwards S. A. Ward R. E. Howells A. M. Breckenridge 《The Journal of pharmacy and pharmacology》1985,37(3):170-174
The plasma pharmacokinetics and mass fate of [14 C]pyrimethamine were investigated in the mouse, following dosage with 12.5, 25, 50, and 75 mg kg?1 (i.p.). Peak plasma concentrations of pyrimethamine were reached between 1 and 2 h and then declined monoexponentially. The mean values for AUC 0 → 30 h increased linearly in relation to the administered dose of pyrimethamine (r = 0.979, P < 0.001). The mean values for intraperitoneal clearance and half-life were not significantly different between dose groups, indicating that the plasma pharmacokinetics of pyrimethamine were independent of dose. The percentage of the administered dose excreted in urine as pyrimethamine (1.3?3.5%) and 14 C-radioactivity (21.7?29.1%) did not change with increasing dose. In contrast, the cumulative percentage of the dose excreted as 14 C-radioactivity in faeces (16.7?22.8%) after the three highest doses 25, 50 and 75 mg kg?1 was significantly less than that seen with the lowest dose of 12.5 mg (50.3%). This suggests extensive biliary excretion of radioactivity, and that the capacity of this process may have been exceeded with the highest doses. Seven days after the administration of each of the three highest doses, a significantly greater percentage of [14 C]pyrimethamine was localized in the soft tissues; i.e. heart, lung and kidney (7.8?13.8%), gut (5.4?9.4%) and particularly the liver (25.0?27.9%) when compared with the lowest dose of the drug (1.2, 1.0, 0.3% respectively). Following each dose, between 85 and 97% of the administered radioactivity was accounted for. These studies indicate, that with higher doses of pyrimethamine, the parent drug and/or metabolites may accumulate in soft tissue, particularly the liver, but without appreciable effects on the plasma disposition and urinary excretion of the drug. 相似文献
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Freund Yvonne R.; Riccio Edward S.; Phillips Sandra J.; Dousman Linda; MacGregor James T. 《Toxicological sciences》1998,42(2):91-98
Increased mortality has been observed when HTV-infected patientswere treated with pyrimethamine (Pyr) as prophylaxis for toxoplasmicencephalitis, suggesting that Pyr might possess im-munosuppressiveactivity. To analyze this in an animal model, immune functionwas assessed in BALB/c mice using a battery of in vivo and exvivo assays and an in vivo model of host resistance to Listeriamonocytogenes infection. Treatment for 30 days with 60 mg/kgPyr decreased circulating white blood cell and lymphocyte countsbut not neutrophil, red blood cell, or platelet counts or hemoglobinlevels. Splenic B cell percentages and lipopolysaccha-ride-inducedB cell proliferation decreased significantly after treatmentwith 60 mg/kg Pyr, as did levels of anti-keyhole limpet hemocyanin(KLH) IgM in serum 7 days after immunization with KLH. Anti-KLHIgG levels 14 days after immunization were not affected. Percentagesof splenic T cells and macrophages and T cell proliferationin the presence of concanavalin A or allogeneic cells were notdecreased by Pyr treatment. An ex vivo assay of T-cell-mediatedcytotoxicity was also unaffected. When host resistance to L.monocytogenes infection was assessed, dramatic increases inmortality were observed in Pyr-treated compared to control mice.Increased numbers of L. monocytogenes organisms were observedin liver and spleen of Pyr-treated mice, compared to controls.The reduction in Listeria resistance, which is T cell mediated,contrasts with the fact that no significant changes in T-cell-mediatedimmunity were observed. It is possible that Pyr affects parametersof innate immunity, which were not monitored in this Study. 相似文献
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Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.
Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.相似文献
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Petrikovics I McGuinn WD Sylvester D Yuzapavik P Jiang J Way JL Papahadjopoulos D Hong K Yin R Cheng TC DeFrank JJ 《Drug delivery》2000,7(2):83-89
This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine. 相似文献