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1.
张小龙孙晓姚晨旭陈洪岩吴启南 《中国药师》2018,(3):518-520
摘 要 目的:建立同时测定肚痛丸中6种成分含量的气相色谱方法。方法: 色谱柱为 HP 5柱 (30 m×0.32 mm,0.25 μm);采取程序升温,载气为氮气,流速为2.0 ml·min-1,进样量为1 μl,分流比为5∶1,进样口温度为280 ℃,检测器(FID)温度为300 ℃。结果:桂皮醛、乙酸龙脑酯、木香烃内酯、去氢木香内酯、厚朴酚、和厚朴酚分别在32.28~516.40 μg·ml-1(r=0.999 3)、27.06~433.00 μg·ml-1(r=0.999 2)、25.65~410.40 μg·ml-1(r=0.999 3)、26.10~417.60 μg·ml-1(r=0.999 3)、24.01~384.20 μg·ml-1(r=0.999 0)、18.32~293.10 μg·ml-1(r=0.999 4)范围内呈良好的线性关系;平均加样回收率分别为99.71%(RSD=0.67%)、99.34%(RSD=1.18%)、100.16%(RSD=0.34%)、100.40%(RSD=0.39%)、99.32%(RSD=1.22%)、99.58%(RSD=0.58%)(n=6)。结论:该方法操作简便,灵敏度高,准确度好,可为控制该制剂的质量提供依据。 相似文献
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摘 要 目的:建立HPLC ELSD同时测定咳灵胶囊中的苦杏仁苷、桃叶珊瑚苷、哈帕苷、贝母辛、贝母素甲和贝母素乙含量的方法。 方法: 采用Ultimate XB C18色谱柱(250 mm×4.6 mm,5 μm),蒸发光散射检测器(漂移管温度105 ℃,氮气流速2.0 L·min-1);以乙腈 甲醇(1〖KG*9〗∶〖KG-*2〗1)与0.4%醋酸溶液为流动相,进行梯度洗脱,流速:0.7 ml·min-1,柱温:35 ℃。 结果: 苦杏仁苷、桃叶珊瑚苷、哈帕苷、贝母辛、贝母素甲和贝母素乙的线性范围分别为13.56~271.20 μg·ml-1(r=0.999 2)、8.48~169.60 μg·ml-1(r=0.999 9)、4.89~97.80 μg·ml-1(r=0.999 7)、2.66~53.20 μg·ml-1(r=0.999 4)、1.82~36.40 μg·ml-1(r=0.999 8) 、2.04~40.80 μg·ml-1(r=0.999 6);平均加样回收率(RSD)分别为97.90%(1.20%),99.21%(1.62%),97.68%(0.75%),98.36%(1.38%),99.70%(0.79%),97.95%(1.56%)(n=6)。结论: 本文建立的方法结果准确,重复性好,样品处理简便,可作为咳灵胶囊的质量控制方法。 相似文献
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摘 要 目的:建立HPLC波长切换法同时测定舒肝益脾液中7个成分。 方法: 色谱柱:Luna C18柱(250 mm×4.6 mm,5 μm);流动相:乙腈 0.05%磷酸溶液,梯度洗脱;流速:0.9 ml·min-1;检测波长:345 nm(滨蒿内酯)、254 nm(毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮和芒柄花素)和210 nm(去氢茯苓酸和茯苓酸);柱温:30 ℃,进样量:10 μl。结果: 滨蒿内酯、毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素、去氢茯苓酸、茯苓酸7个成分的线性范围分别为6.09~152.25 μg·ml-1(r=0.999 9)、2.42~60.50 μg·ml-1(r=0.999 8)、1.61~40.25 μg·ml-1(r=0.999 6)、2.95~73.75 μg·ml-1(r=0.999 4)、6.88~172.00 μg·ml-1(r=0.999 9)、2.55~63.75 μg·ml-1(r=0.999 5)、2.09~52.25 μg·ml-1(r=0.999 9);平均加样回收率分别为98.96%(RSD=1.18%),97.89%(RSD=1.41%),97.18%(RSD=0.88%),96.87%(RSD=0.97%),99.32%(RSD=1.25%),96.77%(RSD=0.86%)和98.55%(RSD=1.03%)(n=9)。结论: 本文建立的HPLC波长切换法同时测定舒肝益脾液中的7个成分,方法简便,可作为舒肝益脾液全面可靠的质量控制方法。 相似文献
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摘 要 目的:建立HPLC法测定盐酸阿莫地喹中4,7-二氯喹啉的残留量。 方法: 采用Agilent ZORBAX SB C18柱(250 mm×4.6 mm,5 μm),以乙腈 0.25%磷酸溶液(80∶20)为流动相,流速为1.0 ml·min-1;柱温为30 ℃;检测波长为228 nm;进样量为10 μl。 结果: 在该色谱条件下,4,7-二氯喹啉杂质峰与主峰能有效分离,空白溶剂不干扰测定,4,7-二氯喹啉的线性范围为0.140 9~14.094 5 μg·ml-1(r=1.000 0),平均回收率为100.14%(RSD=0.32%,n=9)。 结论: 本方法简单,准确,灵敏度高,重复性好,适用于盐酸阿莫地喹中4,7-二氯喹啉残留量的测定。 相似文献
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摘 要 目的:建立抑制电导离子色谱法同时测定浓维磷糖浆中有效成分甘油磷酸根及磷酸根的含量。方法: 采用AG19 HC(50 mm×4 mm)保护住和IonPac AS18 HC(250 mm×4 mm)阴离子分析柱,以氢氧化钾溶液梯度淋洗,检测器为电导检测器,检测方式为抑制电导检测。结果:在该色谱条件下,甘油磷酸根峰与磷酸根峰均能有效分离,线性范围分别为1.054~84.35 μg·ml-1(r=0.999 4)及0.316 8~25.35 μg·ml-1(r=0.999 8);平均回收率分别为99.35%(RSD=1.16%,n=9)和98.96%(RSD=2.61%,n=9)。结论:本法简便,准确,专属性强,有助于更好地控制本品的质量。 相似文献
6.
摘 要 目的:建立RP HPLC双波长法同时测定参莲胶囊中氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱7种生物碱含量。 方法: 采用Venusil XBP NH2(250 mm×4.6 mm,5 μm)色谱柱,以乙腈 0.01%醋酸铵水溶液为流动相梯度洗脱,流速为1.0 ml·min-1,检测波长为210 nm、280 nm。 结果: 氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱线性范围分别为32.07~513.07 μg·ml-1(r=0.998 8)、37.90~606.40 μg·ml-1(r=0.999 2)、23.07~369.07 μg·ml-1(r=0.999 2)、52.37~837.87 μg·ml-1(r=0.999 7)、17.63~282.13 μg·ml-1(r=0.999 1)、5.30~84.80 μg·ml-1(r=0.999 5)、8.87~141.87 μg·ml-1(r=0.999 7);平均加样回收率(n=9)为100.16%~102.84%(RSD≤2.0%)。5批样品中氧化苦参碱、槐定碱、氧化槐果碱、苦参碱、槐果碱、粉防己碱、防己诺林碱含量依次为9.18~9.69 mg·g-1、9.35~11.74 mg·g-1、6.73~7.09 mg·g-1、15.17~15.96 mg·g-1、5.03~5.33 mg·g-1、1.23~1.97 mg·g-1、2.48~2.74 mg·g-1。 结论: 所建立的多成分分析方法可用于参莲胶囊中7个生物碱成分的含量测定。 相似文献
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摘 要 目的:建立加味小柴胡颗粒的质量标准。方法: 采用TLC法对制剂中柴胡、黄芩、黄连进行定性鉴别;采用UPLC法对制剂中甘草苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、甘草酸单铵盐进行定量分析。色谱柱:Aglient ZORBAX Eclipse Plus C18(50 mm×2.1 mm,1.8 μm),流动相:乙腈(A) 0.1%磷酸水(B),流速:0.4 μml·min-1,检测波长: [0~11 min:270 nm;11~12 min:254 nm],柱温:35 ℃,进样量:2 μl。结果: 柴胡、黄芩、黄连的TLC图谱斑点清晰,分离度好;甘草苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、甘草酸单铵盐质量浓度分别在1.764~28.224 μg·ml-1(r=0.999 9)、12.390~198.240 μg·ml-1(r=0.999 7)、2.496~39.936 μg·ml-1(r=0.999 9)、4.200~67.200 μg·ml-1(r=0.999 5)、0.940~15.040 μg·ml-1(r=0.999 9)、1.872~29.950 μg·ml-1(r=0.999 6)浓度范围内线性关系良好;平均回收率分别为103.26%,101.36%,97.66%,103.27%,101.37%,102.44%,RSD分别为0.71%,0.81%,2.53%,1.58%,2.31%,3.34%(n=6)。结论: 所建质量标准能有效控制加味小柴胡颗粒的质量。 相似文献
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摘 要 目的:建立HPLC法测定鼻炎愈合剂中阿魏酸、绿原酸和蒙花苷含量。方法: 以Agilent ZORBAX SB C18柱(250 mm×4.6 mm,5 μm)为色谱柱,流动相为乙腈 0.1%磷酸溶液,梯度洗脱,流速为1.0 ml·min-1,柱温30℃,检测波长326 nm。结果: 绿原酸、阿魏酸、蒙花苷分别在3.039 7~30.396 8 μg·ml-1 (r=0.999 7),3.999 9~39.999 4 μg·ml-1 (r=0.999 9),5.820 7~58.207 2 μg·ml-1(r=0.999 9)范围内与峰面积呈良好线性关系,其平均加样回收率分别为98.92%,100.81%,99.89%,RSD分别为1.00%,1.02%,0.99%(n=6)。结论: 该方法操作简便、准确、重现性好,可用于鼻炎愈合剂的质量控制。 相似文献
9.
摘 要 目的:建立高效液相色谱法同时测定化瘀祛斑胶囊中芍药苷、黄芩苷和黄芩素的含量。方法: 色谱柱为Agilent Zorbax SB C18柱(150 mm×4.6 mm,5 μm);流动相为甲醇 0.1%磷酸溶液,梯度洗脱;流速为1.0 ml·min-1;检测波长为230 nm(0~15 min),277 nm(15~45 min);柱温为25℃;进样量为10 μl。结果: 芍药苷、黄芩苷和黄芩素的线性范围分别为1.295~25.890 μg·ml-1(r=0.999 9)、30.050~601.000 μg·ml-1(r=0.999 9)、1.874~37.480 μg·ml-1(r=0.999 9),平均回收率分别为100.9%,100.3%,99.31%,RSD分别为0.92%,1.30%,0.89%。结论: 该法简便、快捷、结果准确、重复性好、实用性强,可以用于化瘀祛斑胶囊的质量控制。 相似文献
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摘 要 目的:建立高效液相色谱法(HPLC)同时测定根管消毒糊剂中多西环素、甲氧苄啶和醋酸地塞米松的含量。 方法: 色谱柱为Wonda Cract C18(250 mm×4.6 mm,5 μm),流动相为甲醇 0.005 mol·L-1庚烷磺酸钠缓冲溶液(内含0.1%三乙胺)(梯度洗脱),流速1.0 ml·min-1,检测波长240 nm,柱温25℃,进样量20 μl。 结果: 多西环素、甲氧苄啶和醋酸地塞米松的质量浓度分别在61 ~ 1 214 μg·ml-1(r=0.999 5)、57 ~ 1 137 μg·ml-1(r=0.999 7)和2~9 μg·ml-1(r=0.999 2)范围内与峰面积呈良好的线性关系;平均加样回收率及相应RSD分别为99.5%(RSD=1.21%)、100.4%(RSD=1.23%)和100.1%(RSD=1.20%)(n=9)。 结论: 该方法准确度好,精密度高,可用于多西环素、甲氧苄啶和醋酸地塞米松的同时测定。 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
16.
《Critical reviews in toxicology》2013,43(5-6):327-369
AbstractThe uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors. 相似文献
17.
Chang Min Kim Kun Ho Son Sung Hwan Kim Hyun Pyo Kim 《Archives of pharmacal research》1991,14(4):305-310
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
18.
《Expert opinion on investigational drugs》2013,22(1):79-86
Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation. 相似文献
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Alberto García-Lled Javier Gmez-Pavn Juan Gonzlez del Castillo Teresa Hernndez-Sampelayo Mari Cruz Martín-Delgado Francisco Javier Martín Snchez Manuel Martínez-Sells Jos María Molero García Santiago Moreno Guilln Fernando Rodríguez-Artalejo Julin Ruiz-Galiana Rafael Cantn Pilar De Lucas Ramos Alejandra García-Botella Emilio Bouza 《Rev Esp Quimioter》2022,35(2):115
The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation. 相似文献