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1.
高效液相色谱法测定野马追药材中槲皮素和山柰素含量   总被引:2,自引:1,他引:1  
缪亚东  欧阳臻  袁斌 《中国药业》2009,18(10):20-21
目的建立高效液相色谱(HPLC)法测定野马追中槲皮素和山柰素的含量。方法药材经提取水解后,采用HPLC法测定。色谱柱为Kromasil—C18柱(250mm×4.6mm,5μm),流动相为甲醇-0.4%磷酸(60:40),检测波长370nm,流速0.6mL/min,柱温30℃。结果槲皮素质量浓度在6—36μg/mL范围内与峰面积线性关系良好(r=0.9999),平均回收率为97.1%,RSD=1.05%(n=6),山柰素质量浓度在4.8~28.8μg/mL范围内与峰面积线性关系良好(r=0.9995),平均回收率为97.5%,RSD=1.28%(n=6)。结论该方法快速、简便、重现性好,为野马追及其制剂提供了一种简便准确的含量测定方法。  相似文献   

2.
郑琰  李荣华 《中国药业》2008,17(21):27-27
目的用高效液相色谱(HPLC)法测定茶碱麻黄碱片中茶碱与盐酸麻黄碱的含量。方法采用Kromasil C18柱(150mm×4.6mm,5μm),流动相为0.05mol/L磷酸二氢钾溶液-甲醇-三乙胺(72:28:0.2),检测波长为215nm,流速为1.0mL/min,柱温为42℃。结果茶碱质量浓度的线性范围为22.34~111.7μg/mL,r=0.9999(n=6),平均回收率为99.85%,RSD为0.14%(n=9);盐酸麻黄碱质量浓度的线性范围为5.17~25.86μg/mL,r=0.9997(n=6),平均回收率为99.25%,RSD为0.39%(n=9)。结论HPLC法简便易行,结果准确,重现性好。  相似文献   

3.
目的建立测定麻氟滴鼻液中盐酸麻黄碱和地塞米松磷酸钠含量的方法。方法采用高效液相色谱(HPLC)法,色谱柱为Hypersil BDS C18柱(250mm×4.6mm,5μm),流动相为0.025mol/L磷酸二氢钾(加入0.5%三乙胺,用磷酸调节pH值至3.5)-甲醇-乙腈(52:38.4:9.6),流速为0.9mL/min,检测波长为257nm,柱温为40℃。结果盐酸麻黄碱质量浓度在100~600μg/mL范围内与峰面积线性关系良好(r=0.9998),平均回收率为100.54%,RSD=1.0%(n=6);地塞米松磷酸钠质量浓度在10~60μg/mL范围内与峰面积线性关系良好(r=0.9998),平均回收率为100.20%,RSD=1.2%(n=6)。结论HPLC法专属性好,操作简便、快速,结果准确,可用于麻氟滴鼻液的质量控制。  相似文献   

4.
高效液相色谱法测定炎可宁中大黄素和大黄酚含量   总被引:2,自引:0,他引:2  
目的采用高效液相色谱(HPLC)法测定炎可宁片中大黄素和大黄酚的含量。方法色谱柱为Shimadzu C18柱(250mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸溶液(85:15),流速为0.8mL/min,检测波长为254nm。结果大黄素、大黄酚与其相邻质峰能完全分离,大黄素与大黄酚质量浓度分别在0.586~29.300μg/mL(n=0.9999)和1.581~79.050μg/mL(r2=1.0000)范围内与峰面积线性关系良好,平均回收率分别为99.58%和100.40%,RSD分别为1.42%和1.82%(n=6)。结论HPLC法简便、准确、重现性好,能排除其他成分的干扰,可用于炎可宁的质量控制。  相似文献   

5.
隋译  孙菲  赵明 《中国药业》2009,18(21):36-36
目的采用高效液相色谱(HPLC)法测定盐酸二甲双胍肠溶胶囊中盐酸二甲双胍含量。方法以Agilent Eclipse XDB—C18柱(250mm×4.6mm,5μm)为色谱柱,10mmol/L磷酸二氢钾水溶液(用磷酸调pH至3.0±0.05)-甲醇(40:60)为流动相。流速为1.0mL/min,检测波长为233nm。结果盐酸二甲双胍质量浓度的线性范围为5.12—102.40μg/mL,r=0.9996(n=5);平均回收率为99.52%,RSD=0.24%(n=6)。结论HPLC法准确、可靠,重现性好。  相似文献   

6.
易文琳 《中国药业》2007,16(17):25-26
目的采用反相高效液相色谱(RP—HPLC)法测定氯霉素滴眼液中氯霉素的含量及有关物质中二醇物和对硝基苯甲醛的含量。方法采用Phenomsil C18柱(250mm×4.6mm,5μm),以甲醇-水-10%四丁基氢氧化铵溶液(350:635:15)为流动相,流速为1.0mL/min,检测波长为272nm。结果质量浓度线性范围氯霉素为40.0~200.0μg/mL(r=0.9997),二醇物为3.0~15.0μg/mL(r=0.9994),对硝基苯甲醛为1.0~5.0μg/mL(r=0.9997);方法的平均回收率为99.24%,RSD=1.08%(n=6)。结论RP—HPLC法分离效果好,灵敏度高,重现性好,结果准确可靠。  相似文献   

7.
目的建立测定清脑降压片中黄芩苷含量的高效液相色谱(HPLC)法。方法采用Watets2690型高效液相色谱仪,色谱柱为Kromasil C18柱(250mm×4.6mm,5μm),流动相为甲醇-水-冰醋酸(46:54:1),检测波长为276nm,流速1.0mL/min,柱温(30±0.5)℃。结果黄芩苷质量浓度在7.92~39.60μg/mL范围内与峰面积呈良好的线性关系(r=0.9982),平均回收率为97.38%,RSD=1.14%(n=6)。结论HPLC法简便、快速、准确,可有效控制清脑降压片的质量。  相似文献   

8.
吴楠  郑琰 《中国药业》2009,18(14):40-40
目的用高效液相色谱(HPLC)法测定消咳宁片盐酸麻黄碱的含量。方法采用Kromasil C18柱(150mm×4.6mm,5μm),流动相为0.05mol/L磷酸二氢钾(用磷酸调pH至3.0)-甲醇(88:12),流速为1.0mL/min,检测波长210nm,柱温室温。结果盐酸麻黄碱质量浓度的线性范围为24.96—74.88μg/mL,r=0.9999(n=5),平均回收率为98.68%,RSD=0.41%(n=6)。结论HPLC法简便、快速、准确,可用于盐酸麻黄碱的质量控制。  相似文献   

9.
高效液相色谱法测定大七厘散中血竭素含量   总被引:1,自引:0,他引:1  
叶优苗 《中国药业》2008,17(11):35-35
目的建立血竭素的含量测定方法,控制大七厘散的质量。方法采用高效液相色谱(HPLC)法,色谱柱为Hyper Clone BDS C18柱(250mm×4.6mm,5μm),流动相为乙腈-0.05mol/L磷酸二氢钠溶液(35:65),检测波长440nm,柱温35℃,流速1mL/min。结果血竭素高氯酸盐质量浓度在2.96—14.80μg/mL范围内与峰面积线性关系良好(r=0.9998),平均加样回收率为98.54%。RSD=1.36%(n=6)。结论HPLC法方便、快速、准确,可用于大七厘散的质量控制。  相似文献   

10.
目的建立测定血浆样品中万古霉素浓度的高效液相色谱(HPLC)法。方法色谱柱为菲罗门双子星C18柱(150mm×4.6mm,5μm),流动相为50mmol/L磷酸二氢钾溶液-乙腈(91.0:9.0),流速为1.0mL/min,检测波长为230nm,柱温30℃。结果万古霉素质量浓度在5,0~100.0μg/mL范围内与峰面积线性关系良好(r=0.9998),最低检测质量浓度为0.2μg/mL;日内、日间精密度RSD分别为3.1%~3.6%和3.5%~5.6%(n=5);低、中、高3种质量浓度净化回收率分别为64.9%,66.3%,65.6%(n=3),方法回收率分别为100.6%,100.2%,98.9%(n=5)。结论HPLC法快速、简便,结果准确,可用于万古霉素血药浓度监测及体内药代动力学研究。  相似文献   

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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   

14.
In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.  相似文献   

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This article assesses pain within the context of the dose response. A substantial number of studies indicate that the dose response for pain-related endpoints is commonly biphasic, being independent of the type of biological model employed, endpoint measured, or agent tested. The quantitative features of the dose response are also remarkably consistent regardless of the receptor pathway that mediates the nociceptive response, indicating a likely downstream message convergence. These findings have important implications for drug discovery, development, and clinical evaluation.  相似文献   

18.
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.
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19.
Zusammenfassung Mittels Gaschromatographie und Dünschichtchromatographie wiesen die Autoren 11 Substanzen nach, welche durch Injektion oder nach Verabreichung per os in die Kniegelenksynovialflüssigkeit eindrangen. In ihrer Aufstellung konnten sie eine direkte Beziehung zwischen Struktur sowie chemischphysikalischen Eigenschaften der Substanz und ihrer Fähigkeit, aus dem Blut in die Kniegelenksynovialflüssigkeit einzudringen, nicht nachweisen, außer der Tatsache, daß Substanzen mit starker Affinität zu Eiweißstoffen erst in höheren Dosen nachweisbar waren.  相似文献   

20.
The current USP National Formulary contains 65 Monographs for drug formulations containing neomycin. All 65 Monographs prescribe a bioassay for neomycin assay. This bioassay, based on cell culture, is labor intensive, has poor precision, and cannot be adapted for purity or identification. High-performance anion-exchange chromatography with integrated pulsed amperometric detection (HPAE-IPAD), a liquid chromatography technique, has been shown to be suitable for neomycin purity analysis and neomycin assay of an over-the-counter first aid cream (Hanko and Rohrer [17]). Here we propose that an HPAE-IPAD assay can replace the bioassay in the 65 neomycin-containing Monographs. We applied the HPAE-IPAD assay to four neomycin-containing drug products representing the four classes of formulations found in the 65 Monographs, liquid, solid, suspension, and cream. Each drug was analyzed with two chromatography systems, and on 3 separate days. For all products, HPAE-IPAD measurements were precise and accurate with respect to the label concentrations. There was also high accuracy for spike recovery of neomycin from the four drug products throughout 70–150% of the labeled concentration. These results suggest that an HPAE-IPAD assay would be an accurate assay for neomycin, and would be faster and more precise than the current bioassay.  相似文献   

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