巴比妥酸盐、Didropyridin及导眠能的高压电泳

在0.025 M pH 9.0的硼酸盐缓冲液中,于100伏/厘米及约3.0毫安/厘米进行高压电泳,展开20分钟可以将下列药物分离:巴比妥+苯巴比妥+二丙烯巴比妥;巴豆基巴比妥(Crotylbarbitale)+甲基苯巴比妥+烯异丙巴比妥(Aprobarbital);环巴比妥;环已烯巴比妥、didropyridin及导眠能。列出了     

高效毛细管电泳法分析血样尿样中巴比妥类药物

建立了血、尿样品中巴比妥类药物的高效毛细管电泳分离测定方法，测定条件为：运行缓冲液配比：１００ｍｍｏｌ／Ｌ十二烷基硫酸钠－１００ｍｍｏｌ／Ｌ磷酸二氢钠－甲醇－水＝７０∶１５∶５∶１０（ｐＨ值调至７．５５±０．０５），操作电压１７ｋＶ，检测波长２００和２８５ｎｍ，２０ｍｉｎ内７种巴比妥类药物全部得到分离。考察并选择了体液样品的预处理方法，测定了血浆和尿液中６种巴比妥类药物浓度（苯巴比妥、甲基苯巴比妥、异戊巴比妥、硫喷妥、戊巴比妥和速可眠）。测定血药浓度的线性范围为５．０～３５μｇ／ｍｌ，尿样药物浓度线性范围为１．０～８．０μｇ／ｍｌ，最低检测浓度为１．０μｇ／ｍｌ，方法重现性为ＲＳＤ小于１３％。     

急性巴比妥酸盐类中毒85例临床分析

巴比妥酸盐类为临床上常用的鎮靜剂、鎮痙剂及安眠剂。国內常用的有巴比妥、苯巴比妥、异戊巴比妥及戊巴比妥鈉等。急性巴比妥中毒一般多因无意誤服过量或有意吞服过量药物所致。个別中毒患者亦可由于对巴比妥酸盐类药物过敏所引起。急性巴比妥药物中毒的症状以中枢神經系統受抑制为主。昏迷为其主要表現。故临床上凡遇到原因不明的昏迷而有反射消失、肢体松弛等現象均应怀疑有本病之可能。对于有吞服药物史的昏迷患者,更应首先考虑     

酒对药物作用的干扰

酒能直接或间接地引起药物在体内的吸收、代谢、排泄的改变,对药物作用发生干扰,从而影响药物的治疗效果,或产生毒性反应。一、酒与药物并用使药物作用增加 1.巴比妥类:内服巴比妥、戊巴比妥、异戊巴比妥等,如同时饮酒可使巴比妥类中枢抑制作用加强。酒精可增加细胞膜的通透性,使巴比妥类易于进入细胞内而在中枢神经系达到更高浓度;酒精还可改变巴比妥类与脂类及蛋白质的结合。 2.吩噻嚓类:氯丙嗪等与乙醇同时使用可产生药物相加作用,加重中枢抑制作用,产生严重低血压,还可使昏迷加深,甚至发生深度呼吸抑制而死亡。     

抗失眠药的开发和市场动态

早期的失眠治疗药包括苯并二氮革类（如替马西泮、地西泮等）和巴比妥类（如戊巴比妥、丙烯戊巴比妥、异戊巴比妥等）,均会引起副作用,且可能导致成瘾和滥用。苯并二氮革类受体拮抗剂（BZRAs）为γ-氨基丁酸（GABA）激动剂家族成员,在降低成瘾风险方面优势突出,因而成为失眠患者接受治疗的较好选择。率先于20世纪80年代上市的该类药物为Sanofi—Aventis公司产品唑吡坦（zolpidem,Ambien）和佐匹克隆（zopiclone,Imovane）,此后又有许多该类药物陆续面市,包括King制药公司和W1reth公司联合开发的扎莱普隆（zaleplon,Sonata）、Sepracor公司的右佐匹克隆（eszopiclone,Lunesta）和唑吡坦控释制剂Ambien CR。     

六氯对二甲苯对豚鼠肝微粒体药物代谢酶的抑制特性

<正> 前文报道抗华支睾吸虫病药六氯对二甲苯(hexachloro—p—xylene,HCX)对豚鼠肝药酶的抑制作用,HCX能明显延长戊巴比妥催眠时间和血浆戊巴比妥t_(1/2β),并抑制肝匀浆中戊巴比妥侧链羟化酶(pentobarbital side—chain hydroxylase,PSCH)和氨基比林N—脱甲基酶(aminopyrine N—demethylase,ADM)活性。本文在肝微粒体和S9水平,进一步研究了HCX对肝微粒体药物代谢酶的作用,同时对其抑制特性进行了探讨。     

国产异戊巴比妥的杂质分离和结构分析

本文用高效液相半微量制备柱分离出国产异戊巴比妥中的主要杂质，并用紫外、红外、质谱和氢谱等分析技术进行鉴定，杂质为异戊巴比妥的同分异构体：５－乙基－５－（２－甲基丁基）巴比妥酸。     

静心助眠口服液改善睡眠功能试验

目的研究静心助眠口服液对小鼠睡眠功能的影响。方法采用改善睡眠功能检验方法,分别进行了直接睡眠实验、巴比妥钠睡眠潜伏期实验、戊巴比妥钠阈下剂量催眠实验、延长戊巴比妥钠睡眠时间实验。结果本品无明显直接睡眠作用,延长戊巴比妥睡眠时间实验结果为阳性、戊巴比妥钠阈下剂量催眠实验和巴比妥钠睡眠潜伏期实验结果为阴性。结论静心助眠口服液具有改善小鼠睡眠的作用。     

巴比土类药物的催化热滴定法

本文报道,巴比土类药物异戊巴比妥、己烯巴比妥、苯巴比妥、里阿那(Butobarbitone)与司可巴比妥等的催化热滴定法。该法包括分析物的酸碱反应与碱催化指示剂反应,碱催化反应是由丙酮的二聚作用和丙烯     

胃蛋白酶-咖啡因增活消化法提取血和肝中的一些安眠镇静类药物

胃蛋白酶消化生物样品时,合用咖啡因,能使酶的用量减少,消化时间缩短,药物的得率也与常规胃蛋白酶消化法相当或更高。胃蛋白酶—咖啡因增活消化法,已用于兔血和肝中巴比妥、戊巴比妥、苯巴比妥、安定和氯丙嗪浓度的GLC测定。     

气相色谱法鉴别和測定复方茶碱片

本文利用气相色谱法对复方茶碱片的鉴别及含量测定方法进行了研究。该法不需进行任何前处理即可同时鉴别和测定其中六种组分,平均回收率为99.47～102.4%,变异系数0.3～1.4%。该法简便、快速,结果准确。     

气相色谱法测定复方连翘油软胶囊中α-蒎烯与β-蒎烯的含量

目的用气相色谱法测定复方连翘油软胶囊中α-蒎烯与β-蒎烯含量。方法选用玻璃填充柱(3.6mm×2m);涂布3%甲基硅油(OV-17),载气为高纯度氮气,FID检测器。结果α-蒎烯线性范围0.5627~4.5018μg(r=0.9998,n=5),β-蒎烯线性范围1.0724~8.5792μg(r=0.9999,n=5);α-蒎烯平均回收率100.1%,RSD为1.21%(n=6),β-蒎烯平均回收率98.9%,RSD为1.42%(n=6)。结论本法简便、准确、无干扰,可用于复方连翘油软胶囊的质量控制。     

The identification, isolation, and preservation of delta-9-tetrahydrocannabinol (delta-9-THC)

(—)-trans-Δ⁹-Tetrahydrocannabinol (Δ⁹-THC) was isolated from marihuana plant extract, by adsorptive column and glc. The adsorptive column chromatography method consisted of chromatographing marihuana extract on a column packed with a mixture of silica gel (gas chromatography grade (100/120 mesh), silver nitrate and calcium sulphate (CaSO₄·H₂O) (3:1:0·5) with benzene as the eluting solvent. The glc method consisted of chromatographing the extract on a 3 ft silanized glass column (3/8 inch o.d.) packed with 1·5 ft of 2% QF-1 and 1·5 ft of 2% OV-17 on chromosorb W, AW 30–60 mesh, prep grade. A purity of 99% for the isolated Δ⁹-THC was confirmed by infrared spectroscopy, nuclear magnetic resonance, mass spectroscopy. The effects of storage conditions on Δ⁹-THC stability, monitored by glc, indicated the best method for preserving Δ⁹-THC was at 0°, protected from light, stored under nitrogen.     

气相色谱法测定安神补脑液中防腐剂的含量

目的建立安神补脑液中防腐剂的气相色谱方法。方法采用气相色谱法。Agilent7890A气相色谱仪;色谱柱:HP-FFAP石英毛细管柱(柱长30m,内径0.53mm);色谱柱温度:220℃;进样口温度:200℃;分流比为10:1;检测器温度:240℃;自动进样:1μl;载气:N2,流速:5ml/min。结果苯甲酸在0.03991～1.9955mg/ml范围内成线性,回归方程为:Y=1565.1X-53.578,r=0.9991(n=5);对羟基苯甲酸乙酯在0.01019～0.5049mg/ml范围内成线性,回归方程为:Y=1462.4X-5.7411,r=0.9994(n=5)。乙醚提取样品中的苯甲酸和对羟基苯甲酸乙酯,平均回收率为95%～105%,n=9。结论本法操作简便,结果准确,重复性好,可用于安神补脑液中防腐剂的含量测定。     

GLC determination of plasma levels of intact chlorpropamide or tolbutamide.

A GLC procedure was developed for the quantitative estimation of intact chlorpropamide and tolbutamide concentrations in plasma; the drugs are used as mutual internal standards. After extraction of plasma containing the drug and internal standard with toluene, the dried residue is treated with ethereal diazomethane to form the methyl derivatives of tolbutamide and chlorpropamide. Aliquots of the ethereal solution are injected into a gas chromatograph equipped with a glass-lined injection port and glass column packed with a phenyl methyl silicone fluid (OV-25) on Chromosorb W, which facilitates the intact determination of the methyl derivatives of the drugs. The response to the flame-ionization detector was linear over a range of 0.20-25 mug/ml, with a 0.05-mug/ml limit of detectability for both drugs. The method compares favorably with a recently developed high-pressure liquid chromatographic procedure and is adequate for following blood level profiles of single doses of chlorpropamide (125 mg) and tolbutamide (250 mg). Mass spectral evidence showing that intact sulfonylureas are measured is presented.     

5-单硝酸异山梨酯血药浓度测定及其在人的药代动力学

采用气相色谱-电子捕获检测法测定 5-单硝酸异山梨酯的血药浓度。样品经乙醚—正己烷混合溶剂提取,三氟醋酐进行衍生化后,用5% SE-30硅烷化玻璃填充柱分离,以硝酸异山梨酯为内标,⁶³Ni电子捕获检测器检测。此法操作简便,日内、日间误差分别小于4%和6.5%,平均回收率为99.62%±1.19%。在20～800ng·mL^-1血浆浓度范围内呈线性关系(γ=0.9995)。最低检测浓度为2.0ng·mL^-1。应用此法研究了10名健康志愿者单次口服20mg 5-单硝酸异山梨酯片后的药代动力学。     

The estimation of acetylsalicylic acid and salicylate in biological fluids by gas-liquid chromatography

A gas-liquid chromatographic method is described for the simultaneous separation and determination of acetylsalicylic acid (ASA) and salicylic acid (SA) in biological fluids. The salicylates are completely extracted from deproteinized plasma or urine at pH 2 with ether containing p-toluic acid as the internal standard. The silylated derivatives are formed using bis(trimethylsilyl) trifluoroacetamide and separated at 150° on preconditioned 100–120 mesh Gas-Chrom Q coated with 5% OV17 packed into a 6 ft, 1/4 inch o.d. glass column in a gas chromatograph with a flame ionization detector and integrator. Detector response is linear over the range from 0–2 mg ml^?1 for SA and from 0–100 μg ml^?1 for ASA. The time required for the analysis of SA alone or with ASA is about 80 min, the analysis of ASA alone requires about 20 min. The precision of the method is 1 % or better for drug concentrations above 10 μg ml^?1. The limits of detectability for SA and ASA are 1 and 2 μg ml, respectively.     

竹黄多糖SB-Ⅰ及SB-Ⅱ的组成研究——Ⅰ.竹黄多糖SB-Ⅰ及SB-Ⅱ的检定及克分子比测定

将水解后的多糖转化成硅醚衍生物和还原乙酰化衍生物,用气相层析法和气相-质谱法检定了竹黄多糖SB-Ⅰ由L-阿拉伯糖、D-半乳糖、D-葡萄糖组成,竹黄多糖Sb-Ⅱ由L-阿拉伯糖、D-甘露糖、D-半乳糖、D-葡萄糖组成。纸层析未检出阿拉伯糖。采用OV-225固定液的填充柱,对L-阿拉伯糖、D-核糖、D-木糖、L-鼠李糖、D-甘露糖、D-半乳糖、D-葡萄糖七种单糖的还原乙酰化衍生物的分离检定获得满意结果。并在该柱上测定了竹黄多糖组成中的单糖的克分子比。     

A micromethod for the on-column methylation of valproic acid by gas-liquid chromatography

We described a simple procedure for the flash heater methylation of valproic acid and cyclohexylacetic acid (internal standard) by gas-liquid chromatography (GLC). A small volume (100 microL) of sample is acidified with 10% perchloric acid and extracted into hexane. An aliquot is back extracted into 5% tetramethylammonium hydroxide (TMH). A 1 microL sample of the TMH layer is injected into the GLC equipped with flame ionization detector (FID) and a 6 ft x 2 mm i.d. - nickel column packed with 3% OV-17 on 80/100 mesh Supelcoport. The injector temperature is set at 350 degrees C to ensure methylation. Recoveries are greater than 95% of theoretical value. The linearity for calibration points between 15 and 180 microgram/mL is excellent (coefficient of correlation and determination greater than 0.9999). The procedure is rapid and sensitive and does not require a dedicated column in the gas chromatograph.     

挥发油成分的研究——Ⅱ.中国当归与欧当归主要成分的比较

用气相色谱法和气相色谱-质谱法比较了从两种不同方法(已烷提取和水蒸汽蒸馏)所得当归和欧当归挥发油中的主要成分,确定均系藁本内酯(ligustilide)共含量分别约占45%和35%。气相色谱分析是在OV-101和OV-17固定相上进行的,使用火焰电离检测器,氮气作载气。根据两种当归挥发油中主成分相同,提出欧当归可考虑作为当归挥发油制剂的代用品。