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1.
易必新  兰文  李昌亮  王伟姣 《中国药师》2013,(12):1824-1827
目的:建立顶空毛细管气相色谱法测定酚磺乙胺中的乙醇及1,2-二氯乙烷残留量分析方法。方法:采用外标法,DB-624毛细管色谱柱(30 m×0.32 mm,1.80μm),火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。柱程序升温:起始温度40℃,保持6 min,再以10℃·min-1的速率升温至60℃,保持5 min,再以10℃·min-1的速率升温至150℃,保持2 min。载气为氮气;流速为1.0 ml·min-1;分流进样,分流比为5:1。顶空条件:平衡温度65℃,平衡时间为30 min,进样量:1ml。结果:各组分完全分离,线性关系良好(R2〉0.998 0),平均回收率分别为98.84%(RSD=1.79%)和98.92%(RSD=1.26%)。结论:本法简便、准确、精确,适用于酚磺乙胺原料中乙醇和1,2-二氯乙烷残留量的同时检测。  相似文献   

2.
张立光  李扬 《安徽医药》2014,(5):837-840
目的建立测定盐酸乙胺丁醇原料中残留溶剂含量的方法。方法气相色谱法与顶空进样法。色谱柱为DB-624毛细管柱,柱温为50℃,进样口温度为150℃;检测器为FID,温度为200℃;载气为氮气,流速为32 KP;进样量100μL。结果结果表现出了良好的线性关系,甲醇、异丙醇、1,2-二氯乙烷、环己烷检测浓度线性范围分别为2.5~20 mg·L-1(r=0.998 5)、250~1 000 mg·L-1(r=0.998 1)、0.25~2 mg·L-1(r=0.995 3)、2.5~20 mg·L-1(r=0.996 2),平均回收率分别为101.54%、103.66%、103.07%、99.17%,RSD分别为2.1%、1.8%、4.4%、3.8%,最低检测限分别为0.5、25、0.05、0.5 mg·L-1。结论建立的方法简便、灵敏、准确,适用于盐酸乙胺丁醇原料的残留溶剂含量的测定。  相似文献   

3.
目的建立顶空气相色谱法测定卡巴他赛中甲醇、乙醇、丙酮、二氯甲烷和正己烷共5种有机溶剂的残留量。方法采用顶空气相色谱法,氢火焰离子化检测器;载气为氮气,流速为2.0 m L·min-1;色谱柱为DB-624毛细管柱(30 m×530μm,3μm);采用柱温50℃保持7 min,以50℃·min-1的速率升温至220℃,保持3 min;进样口温度为200℃,检测器温度为250℃;分流进样,分流比为5∶1;顶空平衡温度为100℃,顶空平衡时间为20 min;顶空定量环体积为1 m L。以外标法用峰面积计算残留溶剂的含量。结果甲醇、乙醇、丙酮、二氯甲烷和正己烷的线性关系良好(r=0.997 8~0.999 5),平均回收率为94.0%~99.1%,检测限分别为0.67、0.64、0.23、0.94和0.03 mg·L-1。结论本方法可用于卡巴他赛中残留溶剂的检查。  相似文献   

4.
建立毛细管气相色谱法,分别采用溶液直接进样与顶空进样法测定睾酮衍生物AD中溴代环戊烷的残留量。溶液直接进样法:色谱柱为DB-WAX石英毛细管柱,采用程序升温,初始温度50℃,保持5 min;然后以30(℃·min-1)升温至200℃,保持7 min。顶空进样法:顶空瓶加热温度90℃,平衡时间30 min。测得溴代环戊烷分别在4.17~83.4(μg·m L-1)和0.139~2.78(μg·m L-1)范围内呈良好线性关系。回收率分别为100.65%、99.82%。这两种方法均可检测睾酮衍生物AD中溴代环戊烷的残留量,而顶空进样法灵敏度更高,对色谱柱污染较小。  相似文献   

5.
顶空毛细管气相色谱法测定乌拉地尔原料药的溶剂残留量   总被引:2,自引:0,他引:2  
目的:建立乌拉地尔原料药中5种溶剂残留量的毛细管气相色谱测定方法。方法:采用Agilent DB-5毛细管气相色谱柱(30m×320μm×0.25μm),FID检测器,进样口温度200℃,检测器温度230℃;载气为高纯氮气,流速3.0mL.min-1,柱温为程序升温:40℃保持10min,10℃.min-1升温至220℃,保持5min。顶空进样,顶空瓶平衡温度80℃,平衡时间30min。结果:在上述条件下,5种残留溶剂色谱峰的理论板数均大于10 000,相邻峰的分离度均大于2;甲醇、乙醇、丙酮、二氯甲烷、1,2-二氯乙烷的线性关系良好(r分别为0.999 2,0.999 3,0.999 9,0.999 8和0.999 8);最低检出浓度分别为:0.46,0.46,0.23,0.31,0.090μg.mL-1;平均回收率均在90%以上。结论:本方法简单、准确,灵敏度高、重复性好,适用于乌拉地尔原料药中有机溶剂残留量的测定。  相似文献   

6.
目的采用顶空气相色谱法同时测定司坦唑醇原料药中甲醇、乙醇、乙醚、丙酮、异丙醇、乙腈、二氯甲烷、正己烷、正丙醇、乙酸乙酯、四氢呋喃、环己烷和甲苯共13种溶剂残留量。方法采用顶空气相色谱法,色谱柱为DB-624毛细管柱(30 m×0.25 mm,3.0μm),程序升温,进样口温度为200℃,检测器为氢火焰离子化检测器,温度为250℃,载气为高纯氮气,载气流速为2.2 mL·min-1,分流比为10∶1,顶空加热温度为85℃,平衡时间为30 min。结果司坦唑醇原料中13种残留溶剂在各自质量浓度范围内与峰面积线性关系良好(r>0.999);精密度、稳定性试验的RSD均<5.0%,重复性试验中只检出乙醇(RSD<1.0%);平均加样回收率为97.3%~103.8%。结论该方法可用于司坦唑醇原料中13种溶剂残留量的测定。  相似文献   

7.
赵晴  何际芳 《中国药业》2010,19(22):38-39
目的建立测定克林霉素磷酸酯中有机溶剂甲醇、乙醇、丙酮、1,2-二氯乙烷和吡啶残留量的顶空气相色谱法。方法采用AgilentHP-Innowax色谱柱(30 m×0.53 mm,1.0μm),载气为氮气,分流比1∶1,检测器FID温度280℃,柱温80℃,进样口温度200℃,顶空瓶温度80℃,平衡时间40 min。结果甲醇、乙醇、丙酮、1,2-二氯乙烷和吡啶5种溶剂的最低检测限分别为0.06,0.5,0.1,0.005,0.2μg/mL。结论顶空气相色谱法准确、简便、专属性强、重现性好,可作为该产品的质量控制方法。  相似文献   

8.
《中南药学》2017,(4):500-504
目的建立测定吡罗昔康原料及片剂中有机溶剂残留量的方法。方法采用顶空进样毛细管气相色谱法,以二甲基亚砜为溶剂,INNOWAX毛细管柱为色谱柱,氮气为载气,氢火焰离子化检测器,程序升温;顶空瓶平衡温度为90℃,平衡时间为30 min进行测定。结果各有机溶剂均达到基线分离;乙醇、1,2-二氯乙烷、乙苯、对二甲苯、间二甲苯、邻二甲苯、异丙苯、N,N-二甲基甲酰胺的质量浓度在线性范围内与峰面积均呈良好的线性关系(r为0.9991~1.000);平均回收率为88.04%~102.3%,RSD为0.85%~4.8%;检测限为0.05~1.54μg·mL~(-1)。结论该方法操作简便、专属性好、结果准确可靠,可用于控制吡罗昔康原料及片剂中有机溶剂残留量的测定。  相似文献   

9.
目的:建立测定氢溴酸高乌甲素中4种有机溶剂残留量的顶空毛细管气相色谱方法。方法采用DB-624毛细管柱(30 m ×0.53 mm,3μm),程序升温,起始柱温40℃,维持7 min,以25℃·min-1的速率升至200℃,维持1 min;进样口温度:200℃;FID 检测器,检测器温度:250℃;进样方式:顶空进样,平衡温度:80℃,平衡时间:30 min;载气为N2;以DMF为溶剂对氢溴酸高乌甲素中乙醇、乙酸乙酯、三氯甲烷和苯的残留量进行测定。结果4种有机溶剂分离度良好,乙醇、乙酸乙酯、三氯甲烷和苯浓度分别在129.2-1033μg·mL-1(r=0.999)、120.5-964.2μg·mL-1(r=0.999)、3.32-26.5μg·mL-1(r=0.998)、0.14-1.13μg·mL-1(r=0.997)范围内线性关系良好;平均回收率(n=9)分别为97.4%、97.4%、96.8%、98.1%,RSD 分别为1.3%、2.0%、1.7%、3.1%。结论本文建立的顶空毛细管气相色谱法,经方法学验证可用于氢溴酸高乌甲素中有机溶剂残留量的测定,可作为该药质量标准修订的参考。  相似文献   

10.
目的 建立二氯甲烷中三氯甲烷、四氯化碳、1,2-二氯乙烷三种有机挥发性残留杂质的分析方法.方法 采用程序升温气相色谱法进行,运用DB-5色谱柱、电子捕获检测器(ECD),检测器温度为250℃.结果 三氯甲烷、四氯化碳、1,2-二氯乙烷和二氯甲烷间能够完全分离(分离度>3.0),线性范围:三氯甲烷0.5-5.0μg/ml,r=0.997;1,2-二氯乙烷2.7~27.0μg/ml,r=0.999;四氯化碳0.025~0.5μg/ml,r=0.999.平均回收率为:三氯甲烷98.6%;1,2-二氯乙烷103.5%;四氯化碳94.4%.检测限:三氯甲烷0.02μg/ml;1,2-二氯乙烷0.10μg/ml;四氯化碳0.001μg/ml.结论 经方法学验证,该方法灵敏度、准确度均能满足ICH对药品中Ⅰ类、类Ⅱ残留溶剂检测的要求,可用于同时检测二氯甲烷中微量的三氯甲烷、1,2-二氯乙烷和四氯化碳残留.  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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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.
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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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   

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