高效液相色谱法测定阴立爽洗剂中盐酸小檗碱含量

阴立爽洗剂为我院自制制剂,由黄柏、花椒、百部、苦楝皮、苦参、蛇床子、白藓皮、地肤子、鹤虱、枯矾等十余味中药组成,具有清热燥湿,祛风止痒的功效。用于治疗妇科霉菌性、细菌性阴道炎等引起的阴痒、红肿、灼痛等症状。阴立爽洗剂成分复杂,黄柏为方中主药,黄柏有效成分为盐酸小檗碱等多种生物碱[1]。测定其主要有效成分盐酸小檗碱含量的方法有紫外分光光度法[2]、比色法[3]、薄层色谱-荧光分光光度法[4]、双波长薄层扫描法[5]、高效液相色谱法(HPLC)[6]。本实验参考有关资料[7,8],采用HPLC对处方主药黄柏中的盐酸小檗碱建立了含量测定…     

复方石栗喷雾剂的质量研究

目的：建立复方石栗喷雾剂质量控制方法。方法：用TLC及其他化学方法对制剂中黄柏、冰片以及石栗进行鉴别，用紫外分光光度法进行盐酸小檗碱的含量测定。结果：本品定性鉴别色谱及化学方法明显，易于鉴别；小檗碱含量测定线性范围为0．0915-18．3μg，紫外分光光度法测定该制剂中小檗碱（3个不同批号的样品）的平均含量为29．76μg／ml，平均加样回收率为98．72％，RSD为0．85％。结论：紫外分光光度法能准确地测出盐酸小檗碱的含量，结果可靠，适用于基层单位开展检测，但是样品预处理方法较烦琐。     

紫外分光光度法测定盐酸贝那普利含量

目的：探讨盐酸贝那普利的含量测定方法。方法：采用紫外分光光度法测定含量。结果：盐酸贝那普利在240nm处有最大吸收，在10．μg～60．0μg／ml范围内，线性关系良好，平均回收率101．8％，RSD=1．3％。结论：紫外分光光度法测定盐酸贝那普利含量，操作简便，稳定性好，结果准确。     

紫外分光光度法测定注射用甲氨喋呤含量

甲氨蝶呤是医院常用的抗肿瘤药 ,有干扰核酸合成的作用 ,临床用于儿童各类急性白血病、绒毛膜上皮癌、恶性葡萄胎、乳腺癌、卵巢癌、及各种多发性软组织肉瘤等的治疗。其含量测定用ＨＰＬＣ法[1] ,本文用紫外分光光度法测定注射用甲氨蝶呤的含量 ,方法操作简便、测量准确。1　仪器与试药紫外分光光度计岛津ＵＶ - 16 0Ａ型、德国ＳａｄｅｒｉｓＭＣ5微量天平。对照品及其样品、辅料 (由北京医科大学实验药厂提供 ) ,盐酸、碳酸铵均为分析纯 ,实验用水为去离子水。2　实验条件的选择2 1　测定波长的确定　精密称取甲氨蝶呤对照品 10ｍｇ ,用…     

紫外吸收系数法测定盐酸普鲁卡因的含量

目的建立盐酸普鲁卡因注射液中盐酸普鲁卡因的含量测定方法。方法采用紫外分光光度法求出吸收系数，并与药典和文献报道的方法进行比较。结果测定波长290nm，计算公式：盐酸普鲁卡因(g％)=A／E^1% 1cm(取平均系数0.27495)。回归方程：Y=2．424^-3 6．826^-2X，r=0．9999，平均回收率为99．85％，RSD为0．81％(n=4)。结论该测定方法简便、快捷、准确，适用于盐酸普鲁卡因注射液中盐酸普鲁卡因的质量控制。关键词：盐酸普鲁卡因；紫外分光光度法；吸收系数法；含量测定     

盐酸氧氟沙星栓剂的研制及含量测定

本对盐酸氧氟沙星栓的制备方法与含量测定进行了研究。应用紫外分光光度法单波长测定栓剂中盐酸氧氟沙星的含量,平均回收经为99．59％,RSD为1．36％（n＝5）。     

盐酸氨溴索咀嚼片的制备及质量控制

目的介绍盐酸氨溴索咀嚼片的制备及质量控制方法。方法盐酸氨溴索咀嚼片的溶出度测定采用紫外分光光度法,其含量测定则采用高效液相色谱法。结果 盐酸氨溴索咀嚼片的含量测定的线性范围为15~45 mg/L。结论本制剂处方工艺成熟,检测方法简便、准确、可靠,适用于医院制剂室配制和应用。     

三种复方呋麻滴鼻液含量测定方法的比较

目的：对三种复方呋麻滴鼻液含量测定方法进行比较。方法：采用紫外分光光度法,旋光法,滴定法对９ 批样品进行含量测定。结果：紫外分光光度法测定所得结果相对偏差最小。回收率为１０１－７％ , ＲＳＤ为１－２２％ 。结论：采用紫外分光光度法,测定复方呋麻滴鼻液的含量,能得到准确的结果     

紫外分光光度法测定吡嗪酰胺片的含量

目的　建立紫外分光光度法测定吡嗪酰胺片的含量。方法　采用紫外分光光度法 ,测定波长为 2 6 8nm。结果　浓度在 5 .2～ 10 .4 μg·ml-1(r =0 .9999)范围内 ,吸收度值与其浓度呈良好的线性关系 ,方法平均回收率为 99.0 8% ,RSD为 0 .31%(n =6 )。结论　方法简便易行、快速、准确 ,可作为该制剂的质量控制方法     

胃镜润滑剂的质量控制

目的建立胃镜润滑剂质量控制方法。方法以淀粉为黏合剂,甘油为润滑剂,蒸馏水为溶剂,盐酸利多卡因为主药制备胃镜润滑剂,采用紫外分光光度法,测定胃镜润滑剂中盐酸利多卡因的含量。结果盐酸利多卡因的平均回收率为100．42％,RSD为1．09％。结论本制剂制备工艺简便可行,质量稳定可控。     

Abuse of codeine separated from over-the-counter drugs containing acetylsalicylic acid and codeine

Summary In Denmark a new trend concerning the abuse of codeine has been observed. Danish drug abusers have discovered that codeine is easily separated from certain drugs containing acetylsalicylic acid and codeine. When separated the codeine can be used either orally or intravenously. Three different drugs combining acetylsalicylic acid and codeine are available in Denmark, but codeine is only easily separable from one of these. Applying the same procedure to the two other drugs produces unpredictable or unfavourable ratios of codeine to acetylsalicylic acid. In several countries, however, similar drugs combining acetylsalicylic acid and codeine are available. It is not possible from a list of constituents to predict how easily codeine can be separated from a particular drug. Therefore it is strongly recommended that relevant drugs are tested at local forensic laboratories. In case codeine is found to be very easily separated from a product appropriate action should be taken.     

Concentrations of morphine and codeine in urine of heroin abusers

We have measured concentrations of morphine, codeine and 6-monoacetylmorphine in urine of people admitted to the Los Angeles County + University of Southern California Medical Center. Of 60 patients positive for morphine and/or codeine, 10 were judged to be heroin abusers based on positive results for 6-monoacetylmorphine, a specific metabolite of heroin. In nine of these ten patients, 0.028-39.4 microg/ml free codeine and 0.070-307 microg/ml total codeine were detected along with 1.74-218 microg/ml of free morphine and 11.2-2870 microg/ml of total morphine; the morphine-to-codeine ratios were 3.65-228 and 2.27-207 for the free forms and total amounts of these opiates, respectively. In the one patient who was negative for codeine, the concentrations of free and total morphine were 0.114 and 2.22 microg/ml, respectively. Based on our data and literature data available, the following criteria are proposed for judging heroin use from the results of urinalysis, especially when no 6-monoacetylmorphine is detected: (1) a detectable amount of free morphine exists and the concentration of total morphine is higher than 10 microg/ml; (2) a detectable amount of codeine exists; and (3) the morphine-to-codeine ratio is higher than 2 for both the free forms and total amounts of these opiates.     

复方磷酸可待因口服液依赖者多巴胺转运蛋白SPECT显像

目的 研究长期大剂量使用复方磷酸可待因口服液产生依赖对脑纹状体功能的损害.方法 29例复方磷酸可待因口服液依赖者、27例海洛因依赖者和31例健康志愿者分别行99Tcm-2β-[N,N＇-双（2-巯乙基）乙撑二胺基]甲基,3β-（4-氯苯基）托烷（TRODAT-1）SPECT显像,定性分析多巴胺转运蛋白（DAT）影像特征,同时定量分析3组受试者纹状体体积（V,cm3）、质量（m,g）和纹状体与全脑放射性比值（Ra,%）.使用SPSS 13.0软件对3组受试者的V、m和Ra进行t检验.结果 健康对照组双侧纹状体呈典型＂熊猫眼＂形态,DAT放射性分布均匀、对称;复方磷酸可待因口服液依赖者双侧纹状体外形变小,形态失常,放射性分布减低、缺损甚至紊乱,存在部分非特异性放射性分布;海洛因依赖者与其类似.复方磷酸可待因口服液依赖组双侧纹状体V=（23.68±4.94）cm3、m=（24.87±5.19）g、Ra=（5.01±0.88）%,均低于健康对照组的（35.39±4.42）cm3、（37.16±4.64）g和（7.93±0.86）%,t=-9.69,-9.69,-13.01,P均=0.000,高于海洛因依赖组的（18.87±4.66）cm3、（19.81±4.90）g和（4.26±1.02）%,t=3.74,3.74,2.96,P分别为0.000,0.000,0.005.结论 长期大剂量使用复方磷酸可待因口服液产生依赖可破坏纹状体功能,使纹状体部位DAT的分布、密度和活性减低,类似海洛因成瘾性脑病.     

Fatal and severe codeine intoxication in 3-year-old twins—interpretation of drug and metabolite concentrations

This work presents two cases of codeine intoxication in 3-year-old monozygotic twin brothers while treated with a codeine slow-release formulation. One child had to be admitted to the hospital, whereas the other one died at home after aspiration of gastric content. The concentrations of codeine and major metabolites including morphine and corresponding glucuronide conjugates were measured by liquid chromatography–tandem mass spectrometry in serum, urine, cerebrospinal fluid, and brain tissue, respectively. A genetic polymorphism study was carried out in order to determine the ability of the children to metabolize codeine by O-demethylation. A pharmacokinetic calculation was also performed to estimate the administered dose of codeine in question. High concentrations of all substances were found in samples of both children. The pharmacokinetic estimate suggests an overdose of codeine, and the possible reasons for the high opiate concentrations are discussed. Furthermore, the postmortem distribution—during and after resuscitation—might play a major role in the interpretation of postmortem concentration levels.     

Lack of impairment due to confirmed codeine use prior to a motor vehicle accident: Role of pharmacogenomics

BackgroundWe examined forensic serum toxicology and pharmacogenomics data from a woman on codeine shortly before she caused a motor vehicle accident.MethodsA woman driving erratically collided with a parked car of a highway seriously injuring 2 men working to repair the parked vehicle. The woman tested positive for codeine, acetaminophen and barbital. She had been taking these medications for 20 years due to migraine headache. Serum toxicology and genotype analysis for cytochrome P450, UDP glucuronosyltransferase, and other metabolizing enzymes were measured.ResultsThe woman was tried and convicted of driving under the influence resulting in bodily harm and was sentenced to 6 years. Toxicology results on peripheral blood showed a total and free codeine of 840 and 348 μg/L, respectively, and total morphine of 20 μg/L (17, 3, and 0 μg/L for morphine-3-glucuronide, morphine-6-glucuronide, and free morphine, respectively). She was heterozygous for CYP 2D6 *2/*4 (extensive/poor metabolism) and heterozygous for UGT 2B7 *1/*2 (extensive/ultra-rapid metabolism). The woman was also taking fluoxetine and bupropion which are strong inhibitors of CYP 2D6.ConclusionsBased on her genotype and phenotype and reports by the arresting officer, we suggest that the subject in question was not intoxicated by opiates at the time of her motor vehicle accident and may have been falsely incarcerated.     

Evaluation of a method for simultaneous quantification of codeine,dihydrocodeine, morphine,and 6-monoacetylmorphine in serum,blood, and postmortem blood

Summary A solid-phase extraction and gas chromatographic-mass spectrometric method for the simultaneous determination of codeine, dihydrocodeine, morphine, and 6-monoacetylmorphine in serum, blood or postmortem blood is described. The extraction technique allows the determination of free or total morphine (morphine plus morphine glucuronide). Experiments with spiked blood samples resulted in recoveries of 96.4% ± 4.2% for codeine, 95.8% ± 5.1% for dihydrocodeine, 90.3% ± 7.8% for 6-monoacetylmorphine and 92.5% ± 8.1% for morphine. Excellent linearity was obtained over the range 1–1500 ng/mL. The detection limit for all analytes is less than 1 ng/mL.