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1.
常丽 《海峡药学》2016,(5):63-65
目的 建立测定连翘败毒丸中绿原酸和栀子苷的含量的方法.方法 采用高效液相色谱法,以乙腈为流动相A,0.1%磷酸溶液为流动相B,梯度洗脱;检测波长为327nm(绿原酸),238nm(栀子苷),柱温:40℃;流速:1.0mL·min-1;进样量:10μL.结果 绿原酸在7.38μg~73.84μg范围内线性良好(r=0.9999,n=5),栀子苷在6.74μg~67.36μg范围内线性良好(r=0.9999,n =5),平均回收率分别为99.6%和 99.9%,RSD分别为1.1%和1.9%.结论 本方法可用于测定连翘败毒丸中绿原酸和栀子苷含量.  相似文献   

2.
常丽 《海峡药学》2016,(8):93-94
目的 建立测定小儿导赤片中栀子苷和大黄酚的含量.方法 采用高效液相色谱法,以乙腈为流动相A,0.1%磷酸溶液为流动相B,梯度洗脱;检测波长为238nm(栀子苷),254nm(大黄酚),柱温:40℃;流速:1.0mL·min-1;进样量:101μL.结果 栀子苷在6.01μg~120.20μg范围内线性良好(r =0.9999,n=5),大黄酚在1.234μg~24.68μg范围内线性良好(r=0.9999,n=5),平均回收率分别为99.7%和99.7%,RSD分别为0.8%和1.0%.结论 本方法可用于测定小儿导赤片中栀子苷和大黄酚含量.  相似文献   

3.
HPLC法测定栀子柏皮软胶囊中栀子苷和小檗碱的含量   总被引:1,自引:0,他引:1  
目的:建立栀子柏皮软胶囊中指标性成分栀子苷和小檗碱的含量测定方法。方法:采用 Diamonsil ODS-C_(18)柱(5μm,4.6 mm×150 mm);栀子苷的测定以乙腈-水(15:85)为流动相,流速:1.0 mL·min~(-1),检测波长为238 nm;小檗碱的测定以乙腈-0.05%磷酸水溶液-十二烷基硫酸钠(55:45:0.1)为流动相,流速:1.0 mL·min~(-1),检测波长为265 nm。结果:栀子苷的线性范围为10.2~50.3 mg·mL~(-1),平均回收率为96.8%(n=9),RSD 为1.5%;小檗碱在9.5~66.4μg·mL~(-1)浓度范围内线性关系良好,平均回收率为97.4%(n=9),RSD 为1.3%。结论:本方法简便、灵敏,重现性好,适用于栀子柏皮软胶囊的质量控制。  相似文献   

4.
目的:建立同时测定栀子中栀子苷、西红花苷-Ⅰ和西红花苷-Ⅱ含量的方法,并对14批不同产地栀子药材中3种成分的含量进行测定。方法:采用反相高效液相色谱法。色谱柱为Thermo ODSC1(8250mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1.0mL·min-1,检测波长分别为栀子苷238nm、西红花苷-Ⅰ和西红花苷-Ⅱ440nm。结果:栀子苷、西红花苷-Ⅰ、西红花苷-Ⅱ的进样量分别在0.448~5.600、0.142~1.775、0.026~0.325μg范围内与各自峰面积积分值呈良好线性关系,r分别为0.9992、0.9998、0.9999;三者平均回收率分别为99.69%(RSD=2.44%,n=6)、98.26%(RSD=2.62%,n=6)、102.94%(RSD=3.13%,n=6)。结论:本方法简便、准确、重复性好,可同时测定栀子中栀子苷、西红花苷-Ⅰ和西红花苷-Ⅱ的含量。  相似文献   

5.
目的建立快速测定栀子复方制剂复方牛黄消炎胶囊、清胃黄连丸和龙泽熊胆胶囊中栀子苷和西红花苷-1的方法。方法采用UPLC法。色谱柱为BEH C18柱(50mm×2.1mm,1.7μm);流动相:甲醇-水以不同梯度洗脱;流速:0.3mL·min~(-1);检测波长:0~7min为238nm,7~20min为440nm;柱温:30℃;进样量为2μL。结果 3种复方制剂中栀子苷在0.010~1.000mg·mL~(-1)范围内呈良好的线性关系(r=0.999 9),平均回收率分别为98.2%,99.9%和100.3%,RSD分别为1.3%,1.4%和1.0%;西红花苷-1在0.1~10.0μg·mL~(-1)范围内呈良好的线性关系(r=0.999 9)。平均回收率分别为99.6%,97.4%和98.3%,RSD分别为1.3%,1.4%和1.5%。结论栀子苷和西红花苷-1在20min内获得良好分离,该方法简便、准确、快速,可用于栀子复方制剂中栀子苷和西红花苷-1的测定。  相似文献   

6.
罗霄  代琪  谭鹏  文永盛 《医药导报》2013,32(8):1099-1100
目的建立同时测定龙胆泻肝胶囊中龙胆苦苷和栀子苷含量的高效液相分析法。方法采用WatersSunfire C18色谱柱(4.6 mm×250 mm,5μm);乙腈和0.1%磷酸溶液为流动相,梯度洗脱;流速:1.0 mL.min-1;柱温:25℃;检测波长:237和270 nm。结果龙胆苦苷在0.285 8~1.429 0μg(r=0.999 9)、栀子苷在0.402 0~2.010 0μg(r=0.999 8)范围内呈良好的线性关系;龙胆苦苷回收率98.99%(RSD=1.20%),栀子苷回收率99.08%(RSD=0.94%)。结论该方法简便、准确,重复性好,可用于同时测定龙胆泻肝胶囊中栀子苷和龙胆苦苷含量。  相似文献   

7.
越鞠胶囊中香附、栀子TLC鉴别和栀子苷含量测定研究   总被引:5,自引:0,他引:5  
目的:建立越鞠胶囊中香附、栀子的TLC定性鉴别法和栀子苷的高效液相色谱含量测定法。方法;以α-香附酮为对照品,采用正己烷-醋酸乙酯(9:1)为展开剂,在UV254nm下检视,和以栀子苷为对照品,采用氯仿-甲醇(3:1)为展开剂,香草醛硫酸试液为显色剂,分别对越鞠胶囊中香附和栀子进行薄层色谱法定性鉴别。采用Hpersil C_(18)柱(4.6mm×250mm,5μm),甲醇-水(25:75)为流动相,在238nm检测波长下,以HPLC法测定了越鞠胶囊中栀子苷的含量。结果:越鞠胶囊薄层色谱中,α-香附酮和栀子苷斑点清晰,阴性对照无干扰,并改进了药典中定性鉴别方法的某些缺陷。HPLC定量分析中,栀子苷线性范围为 0.30~1.50 μg(r=1.000),平均回收率为103.6%,RSD=1.0%。方法灵敏度高,结果准确,重现性好。结论:分析方法简便可行,可用于该制剂的质量控制。  相似文献   

8.
王子雯  唐灿  孙嘉婧  王刚  黄锐  李希 《药物分析杂志》2012,(9):1554-1558,1563
目的:探索巴中产栀子的最佳采收期和生长期。方法:以HPLC-ELSD法测定巴中产栀子主要有效成分栀子苷、西红花苷Ⅰ、熊果酸含量,并采用t检验和Z-分综合评价法分析数据;测定栀子苷采用Kromasil C18键合硅胶柱(4.6 mm×250mm,5μm),流动相为乙腈-水(10∶90),流速1 mL.min-1,检测波长238 nm;测定西红花苷Ⅰ采用Dionex C18键合硅胶柱(4.6 mm×150 mm,5μm),流动相为甲醇-水(45∶55),流速1 mL.min-1,检测波长440 nm;测定熊果酸采用XDB C18色谱柱(4.6 mm×150 mm,5μm),以乙腈-水(81∶19)为流动相,流速1 mL.min-1,柱温30℃,采用蒸发光散射检测器,漂移管温度60℃。结果:t检验结果表明:巴中产30年生栀子西红花苷Ⅰ含量为红果(成熟期)>黄果(近成熟期)>绿果(未成熟期);栀子苷含量为绿果>黄果>红果;熊果酸含量为绿果>红果>黄果;30年生栀子红果中栀子苷、西红花苷Ⅰ和熊果酸含量均显著高于3年生红果。结论:以栀子苷、西红花苷Ⅰ、熊果酸多指标综合考察巴中产栀子的适宜采收期、生长期,对保证栀子的品质很有意义,也为后续研究提供了依据。  相似文献   

9.
目的:建立同时测定栀子金花丸中栀子苷、盐酸小檗碱和黄芩苷含量的方法,并测定丸中栀子苷的溶出度。方法:采用高效液相色谱法,流动相为甲醇-0.1%磷酸溶液,梯度洗脱,流速为0.8 ml/min,检测波长为254 nm;采用《中国药典》中桨法测定栀子金花丸中栀子苷在水中的溶出量,计算累积溶出度。结果:栀子苷在0.007~0.336μg范围内线性关系良好(r=0.999 9),平均回收率为99.7%,RSD为2.5%;盐酸小檗碱在0.013~0.624μg范围内线性关系良好(r=0.999 8),平均回收率为100.2%,RSD为1.7%;黄芩苷在0.010 5~0.630μg范围内线性关系良好(r=0.999 8),平均回收率为99.0%,RSD为2.3%。栀子苷45 min和120 min累积溶出度分别为79.9%和92.7%结论:建立的方法简便、重复性好,可用于栀子金花丸的质量控制。  相似文献   

10.
目的建立清开灵注射液中测定胆酸、栀子苷、黄芩苷含量的HPLC方法,对不同厂家生产的样品进行质量评价。方法测定胆酸用C_(18) YMC—Pack ODS—A色谱柱,乙腈-水-磷酸(35:65:0.1)为流动相,检测波长192nm;测定栀子苷用C_(18)色谱柱,流动相为乙腈-水(10:90),检测波长238nm;测定黄芩苷用SUPELCO C_(18)色谱柱,甲醇-水-磷酸(47:53:0.2)为流动相,检测波长276nm。结果胆酸平均回收率为97.63%,RSD为1.73%;栀子苷平均回收率为98.15%,RSD为1.64%;黄芩苷平均回收率为99.06%,RSD为1.27%。结论本方法灵敏、准确、简便,可用于清开灵注射液质量控制。  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   

15.
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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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   

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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