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1.
王岩  刘欣欣 《中国药业》2011,20(17):33-35
目的建立测定嘎日迪五味丸中乌头碱、中乌头碱和次乌头碱含量的高效液相色谱法。方法色谱柱为Symmetry C18柱(150 mm×4.6 mm,5μm),流动相为甲醇-水-氯仿-冰醋酸-三乙胺(50∶50∶2∶1∶0.6),柱温为25℃,流速为1.0 mL/min,检测波长为254 nm。结果乌头碱、中乌头碱和次乌头碱的质量浓度均在9.0~45.0μg/mL范围内与峰面积线性关系良好,回归方程分别为A1=2.125×106C+1.252×104,A2=2.143×106C+1.422×104,A3=1.968×106C-2.152×104,相关系数r分别为0.999 6,0.999 8,0.999 8,平均回收率分别为100.40%,99.61%,100.15%,RSD分别为0.72%,0.86%,0.89%。结论所用方法简便、快速、准确,适用于嘎日迪五味丸中乌头碱、中乌头碱和次乌头碱的含量测定。  相似文献   

2.
HPLC测定制川乌中的乌头碱、次乌头碱和新乌头碱   总被引:1,自引:1,他引:0  
目的 建立RP-HPLC测定制川乌中乌头碱、次乌头碱和新乌头碱含量的方法.方法 采用Zorbax Eclipse XDB-C8色谱柱(200 mm ×4.6 mm,5 μm);以20 mmol·L-1三乙胺溶液(磷酸调pH3)-甲醇(95:5)为流动相梯度洗脱;检测波长235nm;柱温30 ℃;流速1.0 mL·min-1.结果 三种生物碱得到有效分离,回归方程分别为:Y乌头碱=1.257×104X+0.222(r=0.9999)、Y次乌头碱=1.302×104X+0.293(r=0.9997)、Y新乌头碱=1.295×104X-0.119(r=0.9999);线性范围为:0.5~20.0μg·mL-1;平均加样回收率分别为98.42%、97.51%、98.33%;RSD分别为1.05%、1.07%、1.05%(n=6).结论 所建方法对制川乌中生物碱的含量控制具参考意义.  相似文献   

3.
目的:建立HPLC-MS分析方法同时测定大鼠血浆中的乌头碱、新乌头碱、次乌头碱含量,并用于研究大鼠口服附子煎液后乌头碱、新乌头碱、次乌头碱的药动学。方法:血浆经氨水碱化后用醋酸乙酯进行液-液萃取。色谱柱为Alltima C18柱(250mm×4.6mm,5μm),流动相为甲醇-10mmol.L-1醋酸铵水溶液(75∶25)。质谱检测方式为选择性离子监测,选择监测的离子为m/z646.45(乌头碱),m/z632.38(新乌头碱),m/z615.64(次乌头碱)和m/z336.60(盐酸小檗碱,内标)。结果:血浆中乌头碱在0.05~5μg.L-1、新乌头碱在0.5~50μg.L-1、次乌头碱在2.5~250μg.L-1范围内线性关系良好,定量限为0.05μg.L-1,血浆中的平均提取回收率高于90%,批内和批间精密度均小于15%。结论:本法灵敏、可靠、简便,适用于乌头碱、新乌头碱、次乌头碱的药动学研究。  相似文献   

4.
目的:探讨中药附子中乌头碱、中乌头碱和次乌头碱的高效液相色谱测定方法.方法:采用HypersilC18(4.6mm×250mm,5.0μm),以甲醇:0.05%磷酸溶液(三乙胺溶液调节pH值6.2)=60:40,检测波长为252nm,柱温为35℃,流速为0.8mL/min.结果:乌头碱回归方程为Y=1.285×103+0.324×102(r=0.9997),在0.261~1.559μg范围内呈较好的线性关系;中乌头碱回归方程为Y=3.354×103+0.015×102(r=0.9996),在0.526~2.031μg范围内线性关系良好;次乌头碱线性回归方程为Y=1.329×103-0.426×102(r=0.9999),在0.152~1.352μg范围内线性关系良好.结论:高效液相色谱法对中药附子中3种有效成分进行测定,方法简单易行,重现性好,精密度高,可作为附子质量控制的方法.  相似文献   

5.
目的 建立RP-HPLC法,测定附子地上部分中新乌头碱和次乌头碱的含量.方法 采用Venusil ABS C18色谱柱(250 mm × 4.6 mm,5 μm),以乙腈-0.1% 乙二胺溶液为流动相,梯度洗脱,柱温30 ℃,流速 1 ml·min-1,检测波长230 nm.结果 新乌头碱、次乌头碱均得到较好分离,分别...  相似文献   

6.
目的:创建高效液相色谱法并对康复新胶囊中新乌头碱、次乌头碱和乌头碱含量进行测定。方法:在氨水的基础上进行乙醚提取,利用OasisMCX固相萃取柱纯化提取液,分析柱是ZORBAX SB-C8(250mm×4.6mm,5μm),流动相是0.04mol·L-1三乙胺(磷酸调pH=3)-甲醇(50∶50),柱温是40℃,检测波长是235nm。结果:在0.002~1μg的范围里,新乌头碱、次乌头碱、乌头碱的线性关系相对较好,回收率超过90%,RSD在2%以下。结论:高效液相色谱法操作相对简便,准确率高,分离效果好,能有效测定康复新胶囊中新乌头碱、次乌头碱和乌头碱含量。  相似文献   

7.
目的建立RP-HPLC同时测定中药乌头不同部位中新乌头碱和乌头碱的含量。方法采用Kromasil C18柱(150 mm×4.6 mm,5μm),以40 mmol乙酸铵缓冲液-乙腈溶液为流动相,梯度洗脱,流速1.0 mL.min-1,检测波长230 nm,柱温30℃。结果新乌头碱、乌头碱分别在2.61~15.66μg、0.26~1.56μg呈良好的线性关系,加样回收率分别为100.4%(RSD=1.2%),98.9%(RSD=0.71%)。结论该方法简便、准确,分离效果好,可用于附子中酯型生物碱的定量分析。  相似文献   

8.
摘 要 目的:建立同时测定活血镇痛膏中的防己诺林碱、粉防己碱、新乌头碱、乌头碱和次乌头碱含量的HPLC梯度洗脱法。 方法: 采用 Dikma C18色谱柱(200 mm×4.6 mm,5 μm),以甲醇-乙腈(3∶1)(A)与0.06%二乙胺水溶液(B)为流动相,进行梯度洗脱,检测波长分别为280 nm(防己诺林碱和粉防己碱)、235 nm(新乌头碱、乌头碱和次乌头碱),流速1.0 ml·min-1,柱温30 ℃,进样量为10 μl。 结果: 防己诺林碱、粉防己碱、新乌头碱、乌头碱和次乌头碱5个成分的质量浓度分别在7.490~149.800、14.610~292.200、4.150~83.000、5.250~105.000、5.140~102.800 μg·mL-1范围内呈良好线性关系,r分别为0.999 9,0.999 8,0.999 2,0.999 6,0.999 9;平均加样回收率(RSD)分别为99.87%(0.49%),97.79%(1.11%),96.97%(1.75%),98.60%(1.50%),97.94%(0.98%)(n=6)。结论:本文建立的HPLC梯度洗脱法能同时测定活血镇痛膏中的5个成分,该方法简便、稳定、可靠,可作为活血镇痛膏全面可靠的质量控制方法。  相似文献   

9.
目的建立强筋健骨丸的含量测定方法。方法以君药制川乌、制草乌中苯甲酰乌头原碱、苯甲酰次乌头原碱及苯甲酰新乌头原碱为目标成分,采用HPLC法,色谱柱Ultimate XB-C_(18)(250mm×4.6mm,5μm);流动相:乙腈(A)-0.1mol·L~(-1)醋酸铵溶液(B);流速:1.0mL·min~(-1);检测波长:235nm。结果苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱质量浓度分别在7.580~121.280(r_1=0.999 9),1.576~25.216(r_2=0.999 8)和7.732~123.712(r_3=0.999 9)mg·L~(-1)范围内线性关系均良好,回收率分别为100.1%,100.0%和99.8%,RSD值分别为0.8%,1.5%和0.6%。结论该方法结果准确、稳定、可靠,能用于强筋健骨丸中苯甲酰新乌头原碱、苯甲酰乌头原碱及苯甲酰次乌头原碱的含量测定,可有效控制产品质量。  相似文献   

10.
目的分析佳蓉片中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、乌头碱和次乌头碱6种乌头类生物碱的含量。方法采用HPLC法。色谱条件:Kromasil C 18色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-四氢呋喃(25∶15)以及0.1 mol·L^-1醋酸铵溶液(每1000 mL加冰醋酸0.5 mL),梯度洗脱;流速为0.8 mL·min^-1;柱温为25℃;检测波长为235 nm。结果苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、乌头碱和次乌头碱分别在4.32~432.40,1.29~128.83,1.08~108.46,1.77~177.30,0.78~78.40和1.19~119.04μg·mL^-1范围内与峰面积线性关系良好;平均回收率分别为96.46%,98.26%,98.03%,98.23%,98.86%和98.70%;RSD值分别为1.50%,1.20%,1.27%,1.06%,1.50%和1.19%;10批制剂中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、乌头碱和次乌头碱的含量范围分别为100.32~119.18,9.35~16.02,7.99~10.87,1.54~1.85,0.87~0.99和2.21~3.27μg·g^-1。结论该方法简单、准确、灵敏、重复性好,可作为佳蓉片中乌头类生物碱成分的定量方法。  相似文献   

11.
乔乐天  刘源  贾号  孙彬 《现代药物与临床》2021,36(12):2502-2506
目的 采用高效液相色谱(HPLC)法同时测定抗妇炎胶囊中木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱10种活性成分。方法 采用InerSustain AQ-C18色谱柱(250 mm×4.6 mm,5 μm),流动相A:乙腈–无水乙醇(80∶20),流动相B:0.1%磷酸溶液,梯度洗脱,检测波长220 nm,体积流量1.0 mL/min,柱温30℃,进样量10 μL。结果 木兰花碱、黄柏碱、药根碱、巴马汀、小檗碱、槐果碱、苦参碱、氧化槐果碱、槐定碱和氧化苦参碱分别在2.69~134.50、1.95~97.50、0.63~31.50、0.86~43.00、11.95~597.50、0.59~29.50、6.08~304.00、4.85~242.50、1.66~83.00、19.79~989.50 μg/mL线性关系良好(r≥0.999 3);平均回收率分别为99.11%、98.23%、96.95%、97.78%、100.02%、97.21%、99.66%、99.52%、98.81%、100.08%,RSD值分别为1.04%、1.23%、1.37%、1.65%、0.70%、1.28%、0.65%、0.81%、1.11%、0.63%。结论 建立的HPLC法可用于抗妇炎胶囊中10种活性成分的测定,作为抗妇炎胶囊质量控制方法。  相似文献   

12.
The minimal inhibitory concentrations (MIC) of erythromycin were determined by broth dilution tests for 313 anaerobic strains, most of which were clinical isolates. All the gram-positive anaerobes tested (84 Peptococcaceae, including 21 Peptostreptococcus anaerobius and 15 Peptococcus variabilis; 65 Corynebacterium acnes and 29 Clostridium strains, including 13 C. perfringens) were sensitive (MIC values 0.012 through 3.12 microgram erythromycin/ml); so were 111 cultures of gram-negative anaerobes (52 Bacteroides fragilis, 12 B. thetaiotaomicron, 7 B. vulgatus, 13 B. oralis, 4 B. melaninogenicus, 10 Sphaerophorus necrophorus, 2 Veillonella sp., 11 members of other species). Erythromycin at concentrations of 6.25 through 200.0 microgram/ml was active against 24 strains (1 B. fragilis, 4 Fusobacterium fusiforme, 9 Sph. freundi, 10 Sph. varius). The present results are compared to the limited number of reports existing with regard to the susceptibility of anaerobes to erythromycin.  相似文献   

13.
14.
Poloxamers are polyoxyethlyene, polyoxypropylene block polymers. The impurities of commercial grade Poloxamer 188, as an example, include low-molecular-weight substances (aldehydes and both formic and acetic acids), as well as 1,4-dioxane and residual ethylene oxide and propylene oxide. Most Poloxamers function in cosmetics as surfactants, emulsifying agents, cleansing agents, and/or solubilizing agents, and are used in 141 cosmetic products at concentrations from 0.005% to 20%. Poloxamers injected intravenously in animals are rapidly excreted in the urine, with some accumulation in lung, liver, brain, and kidney tissue. In humans, the plasma concentration of Poloxamer 188 (given intravenously) reached a maximum at 1 h, then reached a steady state. Poloxamers generally were ineffective in wound healing, but were effective in reducing postsurgical adhesions in several test systems. Poloxamers can cause hypercholesterolemia and hypertriglyceridemia in animals, but overall, they are relatively nontoxic to animals, with LD(50) values reported from 5 to 34.6 g/kg. Short-term intravenous doses up to 4 g/kg of Poloxamer 108 produced no change in body weights, but did result in diffuse hepatocellular vacuolization, renal tubular dilation in kidneys, and dose-dependent vacuolization of epithelial cells in the proximal convoluted tubules. A short-term inhalation toxicity study of Poloxamer 101 at 97 mg/m(3) identified slight alveolitis after 2 weeks of exposure, which subsided in the 2-week postexposure observation period. A short-term dermal toxicity study of Poloxamer 184 in rabbits at doses up to 1000 mg/kg produced slight erythema and slight intradermal inflammatory response on histological examination, but no dose-dependent body weight, hematology, blood chemistry, or organ weight changes. A 6-month feeding study in rats and dogs of Poloxamer 188 at exposures up to 5% in the diet produced no adverse effects. Likewise, Poloxamer 331 (tested up to 0.5 g/kg day(-1)), Poloxamer 235 (tested up to 1.0 g/kg day(-1)), and Poloxamer 338 (at 0.2 or 1.0 g/kg day(-1)) produced no adverse effects in dogs. Poloxamer 338 (at 5.0 g/kg day(-1)) produced slight transient diarrhea in dogs. Poloxamer 188 at levels up to 7.5% in diet given to rats in a 2-year feeding study produced diarrhea at 5% and 7.5% levels, a small decrease in growth at the 7.5% level, but no change in survival. Doses up to 0.5 mg/kg day(-1) for 2 years using rats produced yellow discoloration of the serum, high serum alkaline phosphatase activity, and elevated serum glutamicpyruvic transaminase and glutamic-oxalacetic transaminase activities. Poloxamers are minimal ocular irritants, but are not dermal irritants or sensitizers in animals. Data on reproductive and developmental toxicity of Poloxamers were not found. An Ames test did not identify any mutagenic activity of Poloxamer 407, with or without metabolic activation. Several studies have suggested anticarcinogenic effects of Poloxamers. Poloxamers appear to increase the sensitivity to anticancer drugs of multidrug-resistant cancer cells. In clinical testing, Poloxamer 188 increased the hydration of feces when used in combination with a bulk laxative treatment. Compared to controls, one study of angioplasty patients receiving Poloxamer 188 found a reduced myocardial infarct size and a reduced incidence of reinfarction, with no evidence of toxicity, but two other studies found no effect. Poloxamer 188 given to patients suffering from sickle cell disease had decreased pain and decreased hospitilization, compared to controls. Clinical tests of dermal irritation and sensitization were uniformly negative. The Cosmetic Ingredient Review (CIR) Expert Panel stressed that the cosmetic industry should continue to use the necessary purification procedures to keep the levels below established limits for ethylene oxide, propylene oxide, and 1,4-dioxane. The Panel did note the absence of reproductive and developmental toxicity data, but, based on molecular weight and solubility, there should be little skin penetration and any penetration of the skin should be slow. Also, the available data demonstrate that Poloxamers that are introduced into the body via routes other than dermal exposure have a rapid clearance from the body, suggesting that there would be no risk of reproductive and/or developmental toxicity. Overall, the available data do not suggest any concern about carcinogenesis. Although there are gaps in knowledge about product use, the overall information available on the types of products in which these ingredients are used, and at what concentration, indicates a pattern of use. Based on these safety test data and the information that the manufacturing process can be controlled to limit unwanted impurities, the Panel concluded that these Poloxamers are safe as used.  相似文献   

15.
The physiological disposition of fluvastatin, a potent inhibitor of hydroxymethylglutaryl-CoA reductase and thus cholesterol synthesis, has been studied in the mouse, rat, dog, and monkey using 14C- or 3H-labeled drug. Oral doses of fluvastatin were absorbed at a moderate to rapid rate. The extent of absorption was dose-independent and was essentially complete in all four species studied. However, the drug was subject to extensive presystemic hepatic extraction followed by direct excretion via the bile, thus minimizing the systemic burden and yielding high liver/peripheral tissue concentration gradients for fluvastatin and its metabolites. Only at high doses far exceeding the intended human daily dose of ca 0.6 mg kg-1 did fluvastatin bioavailability approach unity, apparently due to saturation of the first-pass effect. Dose-normalized blood levels of fluvastatin and total radioactivity were higher in the dog than in the other species, suggesting a smaller distribution volume in the former. Fluvastatin was partially metabolized before excretion, the extent of metabolism being smallest in the dog and greatest in the mouse. The half-life of intact fluvastatin ranged from 1-2h in the monkey to 4-7h in the dog. Regardless of the dose or dose route, the administered radioactivity was recovered predominantly in feces, with the renal route accounting for less than 8 per cent of the dose. No tissue retention of radioactivity was observed, and material balance was essentially achieved within 96h after dosing.  相似文献   

16.
A gas-liquid chromatographic method for the simultaneous measurement of bupivacaine, etidocaine, lidocaine, meperidine, mepivacaine, and methadone in serum is described. The drugs and the internal standard, prilocaine, are extracted from 1 ml of serum. The procedure involves a two-step extraction and injection of the extract into a gas chromatograph equipped with a 10-ft OV-11 glass column and a nitrogen-phosphorus detector. The temperature gradient program results in a run time of 16 min and retention times for meperidine, prilocaine (internal standard), lidocaine, etidocaine, mepivacaine, methadone, and bupivacaine of 3.8, 5.4, 6.0, 8.7, 11.0, 11.7, and 14.8 min, respectively. Standard curves for all drugs were linear over the 80 to 2,000-ng/ml range and recovery of all components averaged 97 +/- 2% with the lowest detection limit of 10 ng/ml for all drugs except meperidine and methadone, which were 20 ng/ml. The within-day coefficients of variation ranged from 12 to 8% at 500 ng/ml. The day-to-day coefficients of variation of the slope and intercept values ranged from 2 to 0% and 130 to 3%, respectively. Response factors of the nitrogen-specific collector varied with the drug analyzed and resulted in peak area variation at constant offset and attenuation of 30%. This method is intended and adequate for therapeutic monitoring of chronically treated pain patients who are being given various combinations of local anesthetic and/or narcotic agents.  相似文献   

17.
Background: The introduction and approval of new antiretroviral agents in the US and Canada bring new opportunities and new challenges. Arguably, for the first time ever, clinicians have the drugs necessary to achieve the goal of suppressing HIV RNA to levels less than 50 copies/mL in even the most treatment-experienced patients and in those with extensive drug-limiting resistance mutations. However, the use of these new agents is complicated by many drug–drug interactions and – to some extent – pre-existing mutations. To derive maximum durability from the use of these newer drugs, a thorough understanding of their indications and limitations is critical. Objective: To thoroughly review the six most recently approved or soon-to-be-approved antiretroviral drugs in the US and Canada: tipranavir, darunavir, etravirine, rilpivirine, maraviroc, and raltegravir. Methods: Discussion of the indications for, and pharmacokinetics, resistance profile, activity, toxicity, and clinical trials results of, the six new agents. Results/conclusions: These six new agents have resulted in marked progress towards the goal of being able to provide HIV-infected individuals with the drugs necessary to achieve decades of durable suppression of HIV without substantial toxicity.  相似文献   

18.
马蹄金中铁、钙、镁、铜、锌、锰、镍的形态分析   总被引:6,自引:0,他引:6  
目的:研究马蹄金全草中微量元素的存在形态。方法:采用超声波提取。电感耦合等离子发射光谱法(ICP—AES)对马蹄金不同形态中Fe、Ca、Mg、Cu、Zn、Ma、Ni等元素进行分析。结果:Fe元素在马蹄金中含量最高,而Cu元素含量最低;Ca的提取率最高,Fe的提取率最低;Ca、Mg、Cu、Zn、Mn、Ni6种元素的可溶态均大于悬浮态;且渣中的微量元素含量较高。结论:马蹄金中的微量元素是以无机态为主,多种形态共存的复杂体系。  相似文献   

19.
Soil contaminated with Cd, Pb, Cu, and Zn in the Zhangshi irrigation area is very hard to be remediated. Phytoextraction is considered as an efficient method to remove these toxic metals from soil. In the present study, three vegetables including sugar beet (Beta vulgaris), mustard (Brassica juncea L.), and cabbage (Brassica oleracea L. var. capitata Linn.) were used to bioaccumulate heavy metals in soil through pots experiment for 90 days; and nutrient elements were applied to stimulate the phytoextraction of metals. Results of bioconcentration factors (BCF) and translocation factors (TF) from this study showed that these plants could phytoextract heavy metals, but the accumulation and translocation of metals differed with species of plants, categories of heavy metals, and some environmental conditions (e.g. nutrients). Meanwhile, the addition of nutrient elements, such as N, P, and Fe, could affect the phytoremediation of heavy metals via promoting the normal metabolism of vegetables or changing forms of metals. Results of this study could provide some available information for in-site bioremediation of soil from Zhangshi irrigation area.  相似文献   

20.
The drug habits for 78 confirmed opiate addicts were studied on eight scales from the Process Association Test of Addiction (PATA) for many drug names. Through cluster analysis eight stages of addiction were defined: “to be clean”, “to learn about drugs”, “to hustle”, “to chip” (also “to be high”), to be psychologically dependent or “to need a shot”, “to be hooked”, “to kick a habit” and “to be in treatment”. Associations stimulated by the words heroin and morphine were very similar over the eight stages of addiction in opiate addicts. The subjects were especially inclined to associate morphine and heroin with the most severe level of addiction, “to be hooked”. Associations to both methadone and cocaine were elevated at the “hooked” stage, but in other respects associations to these drugs were opposite. Thus, associations to cocaine were focused on the stage of psychological dependence and the lower intermediate stage of addiction, “to chip” and “to be high”, whereas associations to methadone suggested a turning away from addiction as indicated by avoidance associations (“to come down” and “to kick a habit”) as well as associations to “treatment” and “to be clean”. Marijuana, Benzedrine, “goofball” (barbiturates) and alcohol habits were prominent at an intermediate stage of addiction (“to chip” and “to be high”). Avoidance associations were common for Benzedrine and “goofballs” (also pentobarbital) but not for marijuana or alcohol. “Hustling” associations were frequent for marijuana but not for alcohol.  相似文献   

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