高效液相色谱法同时检测人血清中3种抗癫痫药的浓度

目的　建立一种同时测定人血清中苯巴比妥 (PB)、苯妥英 (PT)和卡马西平 (CBZ) 3种抗癫痫药物的高效液相色谱(HPLC)定量方法。方法　采用C18色谱柱 ;流动相为甲醇 -水 (5 5∶4 5 ) ;内标物为巴比妥 (BB) ;检测波长为 2 2 0nm ;流速为 1 0ml·min-1;柱温为 30℃。结果　PB在 1 0～ 80mg·L-1范围内呈线性 (r =0 9999,n =5 ) ,PT在 1 0～ 5 0mg·L-1范围内呈线性 (r=0 9996 ,n =5 ) ,CBZ在 0 5～ 2 0mg·L-1范围内呈线性 (r =0 9995 ,n =5 ) ;其最低检测浓度分别为 0 2 5、0 2 5及 0 1mg·L-1;平均回收率分别为 95 75 %、96 5 4 %和 92 13% ;日内RSD(% )小于 6 2 9% ,日间RSD(% )小于 6 6 4 % (n =5 )。结论　本法简便、快速、灵敏 ,适用于癫痫病人血药浓度监测及药代动力学研究。     

RP-HPLC法测定人血浆中苯巴比妥、苯妥英和卡马西平浓度

目的建立血浆中苯巴比妥(phenobarbital,PB)、苯妥英(phenytion,PT)和卡马西平(carbamazepme,CBZ)三种抗癫痫药的HPLC检测方法.方法采用日本分光JASCO-1500系列高效液相色谱仪,ODS Hypersil柱(150 mm×4.6 mm,5 μm),以艾司唑仑(estazolam,EZ)为内标,流动相组成为甲醇-乙腈-水-四甲基乙二胺-冰醋酸(50:50:100:2:1.5),流速为O.8ml@min,紫外检测波长254 nm,灵敏度AuFs=O.02.结果血浆中3种组分和内标均能很好地分离,无明显的干扰峰.PB线性范围为2～50 mg@L-1,r=O.9997;PT线性范围为2～50 mg@L-1,r=O.9998;CBZ线性范围为O.5～20mg@L-1,r=O.9998,日内、日间RSD＜5%.结论本法操作简便、结果可靠,适用于药物监测和中毒分析.     

PLC法测定血浆中喷昔洛韦浓度

目的 :建立泛昔洛韦人体内活性代谢产物—喷昔洛韦血浆浓度测定方法。方法 :采用C18反相色谱柱 ,以0 0 2mol·L-1高氯酸 -甲醇 (4 5 0∶8)为流动相 ,荧光检测波长为λex=2 70nm ,λem=375nm ,内标物为阿昔洛韦 ,血浆样品采用 6mol·L-1高氯酸液沉淀蛋白。结果 :喷昔洛韦血浆浓度在 0 12 5～ 16mg·L-1范围内 ,与面积呈良好的线性关系 (r=0 9998) ;本试验最低检测浓度为 0 0 5mg·L-1,日内及日间RSD均小于 8% ,喷昔洛韦的方法回收率大于 90 %。结论 :该方法简便、准确、灵敏 ,可用于泛昔洛韦人体药代动力学及生物利用度的研究     

高效液相色谱法测定克林沙星血药浓度

目的 :建立用高效液相色谱法测定血浆中克林沙星浓度的方法。方法 :血浆样品在酸性条件下 ,以Oasis小柱提取环丙沙星为内标 ,采用LichrosorbC18(5 μm)柱 ,流动相为乙腈 - 0 0 5mol·L-1柠檬酸三乙胺溶液 (pH 2 5 ) (2 0∶80 ) ,流速为 1 0mL·min-1,检测波长 30 0nm ,克林沙星和内标的保留时间分别为 7 1min和 4 5min。结果 :线性范围在 0 0 3～10 μg·mL-1(r=0 9998) ,最低检测浓度为 0 0 2 μg·mL-1,RSD <7%。用本法测定了 6只大鼠灌胃剂量 5 0mg·kg-1克林沙星后血浆中克林沙星的浓度经时变化过程。结论 :本方法可用于克林沙星的血药浓度测定及药代动力学研究。     

HPLC法测定人血清中丙戊酸的含量

目的 　建立柱前衍生 HPLC法测定血清样品中丙戊酸钠的含量。 方法 　以 Nova-pak C1 8( 3 .9× 15 0 mm)为色谱柱 ,流动相为甲醇 -水 ( 78∶ 2 2 ) ,检测波长为 2 45 nm。样品酸化提取后经α-溴苯乙酮衍生化后分析 ,环己烷羧酸为内标。结果 　线性范围为 5～ 2 5 0 mg· L- 1 ,r=0 .9998;平均回收率为 98.78% ,日内、日间 RSD均小于 3 .2 2 % ,最低检出浓度为 0 .0 8mg· L- 1 。 结论 　本法适用于 VPA的血药浓度测定。     

RP-HPLC测定母体及胎儿血浆中罗哌卡因和布比卡因的药物浓度

目的 :建立罗哌卡因、布比卡因血浆药物浓度的反相高效液相 (RP HPLC)测定方法 ,并测定其母体和 (或 )胎儿血药浓度 ,为临床合理用药提供参考。方法 :采用AgilentHPLC系统 ;色谱柱 :Dikma C18(5 μm ,4 .6× 15 0mm)。以罗格列酮作为内标 ,流动相为磷酸二氢钠缓冲液 (10mmol·L- 1,pH3.0 )∶乙腈 =78∶2 2 ,流速 1.0mL·min- 1,λ =2 10nm。结果 :罗哌卡因线性关系为Y =0 .0 2 95X -0 .0 2 98(n =7,r =0 .9998) ;最低检测浓度为 0 .0 1mg·L- 1;平均回收率为 99.82 % ;日内、日间RSD分别小于 2 .4 7% ,3.75 % ;布比卡因线性关系为Y =0 .0 2 87X + 0 .0 2 71(n =7,r =0 .9998) ;最低检测浓度为 0 .0 1mg·L- 1;平均回收率为 10 1.0 1% ;日内、日间RSD分别小于 2 .6 9% ,4 .75 %。测定 6 0个血样 ,罗哌卡因浓度为 0 .15～ 0 .7mg·L- 1,布比卡因为 0 .1～ 0 .5 8mg·L- 1。结论 :RP HPLC法简便、灵敏、准确 ,可以用来测定临床血样中罗哌卡因、布比卡因的药物浓度 ,可为临床合理用药提供参考。     

高效液相色谱法测定人血液和尿中帕尼培南-倍他米隆的浓度

目的 :建立高效液相色谱法测定人血浆及尿样品中帕尼培南 (panipenem ,PAPM)、倍他米隆(betamipron,BP)浓度。方法 :以 1mol·L-1MOPS(pH 7.0 )为稳定剂 ,PAPM浓度测定采用外标法 ,BP则采用内标法 ,内标物为N 苯甲酰 DL 丙氨酸。PAPM测定的色谱条件 :色谱柱为C18Diamosil(TM ) (2 5 0× 4.6mm ,5 μm) ;血浆中流动相为CH3 OH∶0 .0 4mol·L-1CH3 COONH4(pH 4.0 ) / 5∶95 ,尿中流动相为CH3 OH∶ 0 .0 4mol·L-1CH3 COONH4(pH 4.0 ) / 2∶98;检测波长为 2 99.3nm ;流速为 1 .6mL·min-1。BP测定色谱条件 :色谱柱同PAPM ;血浆中流动相为CH3 CN∶CH3 COOH∶H2 O/ 2 0∶1∶79,尿中流动相为CH3 CN∶CH3 COOH∶H2 O/ 1 2∶1∶87;检测波长为 2 40nm ;血浆中流速为1 .4mL·min-1,尿中流速为 1 .6mL·min-1。结果 :血浆中PAPM在 0 .5～ 5 0 .0mg·L-1范围、BP在0 .2～ 5 0mg·L-1范围内具良好线性关系 (r =0 .9999) ;尿中PAPM和BP在 2～ 2 0 0mg·L-1浓度范围内具良好线性关系 (r =0 .9999)。PAPM和BP平均方法回收率为 1 0 1 .69% ;日内、日间精密度RSD均 <5 %。结论 :本方法简便、快捷、灵敏、准确 ,适用于临床药动学及药效学的研究     

RP-HPLC同时测定血浆中苯巴比妥、苯妥英、卡马西平和氢化可的松的浓度

目的　建立同时测定人血浆中苯巴比妥 (PB)、苯妥英 (PHT)、卡马西平 (CBZ)和氢化可的松 (HC)浓度的方法。方法　采用C18柱 (15 0mm× 4 6mm ,5 μm) ,以 0 0 1mol·L-1NaH2 PO4(pH 3 0 ) -甲醇 -乙腈 (4 7∶4 9∶4 )为流动相 ,莫沙必利为内标 ,检测波长 2 4 5nm。结果　标准曲线线性范围PB为 12 5～ 2 0 0 0 μmol·L-1,PHT为 6 2 5～ 10 0 0 μmol·L-1,CBZ为 5 0～ 80 0 μmol·L-1,HC为 80～ 12 80 μg·L-1。萃取回收率PB为 77 95 %～ 87 83% ,PHT为 84 97%～ 86 4 5 % ,CBZ为 79 2 1%～ 93 36 % ,HC为82 90 %～ 93 36 % ;方法回收率PB为 97 2 8%～ 10 0 5 % ,PHT为 96 4 3%～ 10 0 4 2 % ,CBZ为 95 6 3%～ 10 0 4 2 % ,HC为 98 82 %～10 0 98% ;日内测定RSD则分别为 1 2 1%～ 5 95 %、0 6 5 %～ 5 5 2 %、3 4 %～ 9 9%、1 70 %～ 6 0 3% ;日间测定RSD则分别为1 17%～ 6 76 %、3 6 4 %～ 7 2 6 %、0 96 %～ 4 81%、1 4 4 %～ 7 4 2 %。结论　本法快速、灵敏、准确 ,可用于临床同时监测 4种药物的浓度     

反相高效液相色谱法测定卫肺特片中3组分的含量

目的 :建立反相高效液相色谱法 (RP HPLC)测定卫肺特片中利福平、异烟肼、吡嗪酰胺的含量。方法 :采用HypersilC18色谱柱 ,流动相为甲醇 pH 4 .5磷酸盐缓冲液 (70∶30 )和甲醇 pH 3.0磷酸盐缓冲液 (8∶92 ) ,检测波长 2 6 2nm。结果 :线性范围、回收率分别为 :利福平 3.0 1～ 18.0 6mg·L-1(r =0 .9999) ,10 0 .5 % (RSD为 1.0 % ) ;异烟肼 6 .2 4～ 2 1.84mg·L-1(r =0 .9998) ,10 0 .5 % (RSD为 1.3% ) ;吡嗪酰胺 2 4 .72～ 86 .5 2mg·L-1(r =0 .9999) ,99.6 % (RSD为 0 .6 % )。结论 :该方法可同时测定卫肺特片中 3组分的含量     

高效液相色谱法测定依托度酸及其在大鼠的药动学(英文)

目的 :建立测定依托度酸浓度的高效液相色谱法并研究该药在大鼠体内的药动学。方法 :血浆 2 0 0 μL加入 1 0 0mg·L-1 内标 (奥沙普秦) 50 μL ,酸化后用乙酸乙酯∶正己烷 (1∶1 9)提取。采用C1 8分析柱 ,以乙腈∶水∶三乙胺 (1 6∶84∶0 .0 0 2 )为流动相 ,流速为 1 .0mL·min-1 ;检测波长 2 80nm。大鼠按依托度酸 2 0mg·kg-1 剂量灌胃 ,给药前及给药后 5 ,1 0 ,2 0 ,30min和 1 ,3,6 ,1 2 ,2 4 ,48,72h采血 ,测定血浆药物浓度。绘制血药浓度 -时间曲线图并计算主要药动学参数。结果 :依托度酸与内标物的保留时间分别为 5 .2 8min和 6 .80min ;依托度酸浓度在1 .0～ 1 0 0 .0mg·L-1 范围内与依托度酸/内标物的峰面积比呈良好线性关系 ,回归方程为 :Y =0 .0 32 2 7C +0 .0 0 1 2 8,r =0 .9999,n =7。本法高、中、低浓度的绝对回收率为 73 .4 %～ 80 .5 % ,方法回收率在 97.3%～1 0 6.0 % ,日内RSD <4% ,日间RSD <8%。依托度酸的药动学参数为Tmax=0 .2 8h± 0 .1 3h ;Cmax=69mg·L-1 ± 5mg·L-1 ;T1 /2 =1 6 .9h± 2 .1h ;AUC =2 31 4mg·h·L-1 ±32 8mg·h·L-1 。结论 :本法快捷、灵敏、准确、重复性好 ,适用于依托度酸血药浓度测定及药动学研究。     

Safety assessment of poloxamers 101, 105, 108, 122, 123, 124, 181, 182, 183, 184, 185, 188, 212, 215, 217, 231, 234, 235, 237, 238, 282, 284, 288, 331, 333, 334, 335, 338, 401, 402, 403, and 407, poloxamer 105 benzoate, and poloxamer 182 dibenzoate as used in cosmetics

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.     

HPLC法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

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。     

欧洲刺柏（Juniper）

活性成分与药理作用欧洲刺柏药用部位是其浆果，具有促水排泄、防腐、抗胃肠胀气和抗风湿作用，还可改善胃功能。用作促水排泄药可增加尿量（水丢失），但不增加钠排泄。成分萜品烯-4-醇可增加肾小球滤过率，但刺激肾。欧洲刺柏浆果对单纯疱疹病毒体外显示抗病毒活性，并具抗真菌活性。动物实验显示，欧洲刺柏浆果提取物具有堕胎、抗生育、抗炎、抗胚胎植入、降血压、升血压和降血糖作用。欧洲刺柏浆果油具有兴奋子宫的活性，以及利尿、胃肠道抗菌和刺激作用，该油对平滑肌有阻止解痉作用。     

Arformoterol: (R,R)-eformoterol, (R,R)-formoterol, arformoterol tartrate, eformoterol-sepracor, formoterol-sepracor, R,R-eformoterol, R,R-formoterol

Sepracor in the US is developing arformoterol [R,R-formoterol], a single isomer form of the beta(2)-adrenoceptor agonist formoterol [eformoterol]. This isomer contains two chiral centres and is being developed as an inhaled preparation for the treatment of respiratory disorders. Sepracor believes that arformoterol has the potential to be a once-daily therapy with a rapid onset of action and a duration of effect exceeding 12 hours. In 1995, Sepracor acquired New England Pharmaceuticals, a manufacturer of metered-dose and dry powder inhalers, for the purpose of preparing formulations of levosalbutamol and arformoterol. Phase II dose-ranging clinical studies of arformoterol as a longer-acting, complementary bronchodilator were completed successfully in the fourth quarter of 2000. Phase III trials of arformoterol began in September 2001. The indications for the drug appeared to be asthma and chronic obstructive pulmonary disease (COPD). However, an update of the pharmaceutical product information on the Sepracor website in September 2003 listed COPD maintenance therapy as the only indication for arformoterol. In October 2002, Sepracor stated that two pivotal phase III studies were ongoing in 1600 patients. Sepracor estimates that its NDA submission for arformoterol, which is projected for the first half of 2004, will include approximately 3000 adult subjects. Sepracor stated in July 2003 that it had completed more than 100 preclinical studies and initiated or completed 15 clinical studies for arformoterol inhalation solution for the treatment of bronchospasm in patients with COPD. In addition, Sepracor stated that the two pivotal phase III studies in 1600 patients were still progressing. In 1995, European patents were granted to Sepracor for the use of arformoterol in the treatment of asthma, and the US patent application was pending.     

Strength of drug habits: For heroin,morphine, methadone,alcohol, barbiturates,pentobarbital, benzedrine,cocaine, and marijuana

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.