高效液相色谱法测定异福酰胺片的含量

为控制异福酰胺片剂质量,采用HPLC法测定异福酰胺片中异烟肼、利福平和吡嗪酰胺的含量。利福平选择极性较小的流动相,乙腈:0.05mol·L~(-1)磷酸二氢铵(40:65);异烟肼和吡嗪酰胺选择极性较大的流动相,乙腈:0.05 mol·L~(-1)磷酸二氢铵(2:98);均采用C_(18)柱,紫外检测器,检测波长分别为334nm和263nm。利福平、异烟肼和吡嗪酰胺的回收率分别为99.9%、99.8%和99.5%,RSD分别为1.33%、0.5%和1.1%。异烟肼、利福平及吡嗪酰胺日内RSD分别为2.78%、1.62%及1.31%,日间RSD分别为3.84%、2.12%及1.98%,其最低检出量分别为35μg、50μg及25μg。结果表明,采用HPLC法测定异福酰胺片的含量具有各种成分互不干扰,结果准确等特点。     

HPLC法测定双黄连胶囊中连翘酯苷A及连翘苷的含量

目的:建立中成药双黄连胶囊中连翘酯苷A及连翘苷的含量测定方法.方法:采用Phenomenex-ODS-C18(250 mm×4.6 mm,5 um)柱,以甲醇(含1%的四氢呋喃)-水(含0.01 mol·L-1磷酸二氢钾,PH 3.2)为流动相进行梯度洗脱,检测波长280 nm.结果:连翘酯苷A及连翘A的线性范围分别为7.8～139.5μg·ml-1和2.6～47.7μg·ml-1,其线性关系良好.连翘酯苷A平均回收率为100.3%,RSD为0.75%;连翘苷平均回收率为99.2%,RSD为1.03%.结论:该方法准确可靠,可用于本制剂的质量控制.     

用柱前衍生化法测定异福酰胺片中异烟肼的血药浓度

目的 :建立测定血浆中异烟肼浓度的反相高效液相色谱法。方法 :采用C18BDS柱 ,流动相为 0 .0 2mol·L-1磷酸二氢钾∶乙腈 (6 9∶31)。 2 0 0 μl血浆用 2 0 %三氯醋酸沉淀蛋白后 ,上清液加桂皮醛衍生化后直接进样。 结果 :本方法在 0 .1～ 13.88μg·ml-1范围内线性良好。日内和日间误差均小于 10 % ,方法回收率 >95 %。结论 :此方法具有操作简便、灵敏度较高、无干扰等特点 ,已经应用于异福酰胺片人体生物利用度的研究     

离子对反相高效液相色谱法测定异福酰胺片中异烟肼及吡嗪酰胺含量

目的:建立用离子对反相HPLC法同时测定异福酰胺片中异烟肼、吡嗪酰胺的含量.方法:反相高效液相色谱法.色谱柱为μBondapak C18色谱柱(10μm,4.6 mm×250 mm),流动相为乙腈-0.1%庚烷磺酸钠-水(10:30:60),pH2.5,检测波长254 nm,流速:1.0 ml·min-1.外标法测定异烟肼、吡嗪酰胺的含量.结果:线性范围为异烟肼和吡嗪酰胺分别在0.013～0.06mg·ml-1和0.04～0.18mg·ml-1范围内线性关系良好.异烟肼平均回收率99.3%(RSD 0.30%),吡嗪酰胺99.2%(RSD0.3%).结论:本方法准确、快速、可靠、灵敏,可作为该制剂质量检验方法.     

高效液相色谱法测定盐酸奈福泮片的含量

目的:建立盐酸奈福泮片中盐酸奈福泮含量的HPLC测定方法.方法:采用Dikma C18柱(150mm×4.6mm,5μm),以0.01mol·L-1庚烷磺酸钠溶液(稀磷酸调节pH为3.0)-乙腈(67:33)为流动相,流速:1.0ml·min-1;检测波长215nm;柱温:40℃.结果:线性范围为5～35μg·ml-1(r=0.999 8);平均回收率为98.9%,RSD为0.7%(n=6).结论:方法操作简便,快速准确.     

高效液相色谱法测定阿奇霉素片的含量

用高效液相色谱法,测定阿奇霉素片的含量.固定相:十八烷基硅烷键合硅胶(5μm).流动相:0.1mol·L-1磷酸二氢铵溶液(三乙胺调节pH6.5)-乙腈(70∶30);流速:1.0ml·min-1;检测波长210nm,进样量20μL.在选样量2.5～80.0 μg的范围内,进样量与峰面积线性关系良好Y=32798 95934X(r=0.9999),重复进样RSD=0.29%,平均回收率为98.22%.     

HPLC法测定复方硫酸锌滴眼液中盐酸小檗碱和尼泊金乙酯的含量

目的:用HPLC法测定复方硫酸锌滴眼液中盐酸小檗碱和尼泊金乙酯的含量.方法:采用Symmetry Shield RP C18色谱柱(250mm×4.6mm,5μm);以0.033mol·L-1磷酸二氢钾(KH2PO4)溶液-乙腈(60:40)为流动相,检测波长256nm.结果:盐酸小檗碱和尼泊金乙酯在线性范围分别为6.3～37.6μg·ml-1(r=0.9999)和1.9～11.3μg·ml-1(r=0.9999),平均回收率分别为99.9%(RSD=0.7%)和99.3%(RSD=1.2%).结论:本方法简便、准确,可用于该制剂中盐酸小檗碱和尼泊金乙酯的含量测定.     

高效液相色谱法测定口腔溃疡糊剂中盐酸金霉素的含量

目的:建立HPLC法测定口腔溃疡糊剂中盐酸金霉素含量。方法:色谱柱为KF-C18柱(4.6 mm×250 mm,10μm);柱温:40℃;流动相为水-N,N二甲基甲酰胺-乙腈(68:27:5),含磷酸氢二钠0.006 3 mol·L-1和乙二胺四乙酸二钠0.01 mol·L-1,并以10 mol·L-1氢氧化钠溶液调节pH至8.5;检测波长为380 nm。结果:盐酸金霉素在10～100μg·ml-1的范围内线性关系良好,r=0.999 6,平均回收率为99.4%,RSD为1.4%。结论:本方法简便,快速,准确,可用于口腔溃疡糊剂的质量控制。     

高效液相色谱法测定复方呋喃西林滴鼻液中主药的含量

目的:建立高效液相色谱法(HPLC)测定复方呋喃西林滴鼻液中呋喃西林和盐酸麻黄碱的含量.方法:采用HPLC,Agilent Eclipse×OB-C8色谱柱,乙腈:0.05 mol·L-1磷酸二氢钾溶液(22:78)为流动相,检测波长为255 nm.结果:呋喃西林在8～32μg·ml-1浓度范围内,盐酸麻黄碱在400～1600μg·ml-1浓度范围内,峰面积与浓度呈良好的线性关系,其相关系数分别为r=0.999 8和r=0.999 9,呋喃西林的平均回收率为99.66%(RSD为0.68%),日内RSD为0.38%;日间RSD为1.25%;盐酸麻黄碱的平均回收率为99.90%(RSD为0.44%),日内RSD为0.29%,日间RSD为1.12%.结论:本法简便、快速、结果准确,可用于测定复方呋喃西林滴鼻液的含量.     

复合氨基酸胶囊中水溶性维生素的含量测定

目的:建立复合氨基酸胶囊中5种水溶性维生素的含量测定方法.方法:采用高效液相色谱法,用乙腈与庚烷磺酸钠-磷酸钠的水溶液(pH=3.0)为流动相,流速1.0ml·min-1,色谱柱为C18(4.6×250mm,5μm),柱温40℃,检测波长为280nm,进样量为20μl.结果:维生素Bl、维生素B2、维生素B6、维生素C和烟酰胺分别在24.7～75.2μg·ml-1、15.0～44.9μg·ml-1、12.2～37.5μg·ml-1、99.2～299.9μg·ml-1和100.3～300.9μg·ml-1范围内呈线性关系,相关系数均为1.000,平均回收率均在100%±2%范围以内.RSD分别为0.19%、0.26%、0.46%、1.17%和0.52%.结论:本方法准确,简便,快捷,可以同时测定复合氨基酸胶囊中维生素B1、维生素B2、维生素B6、维生素C和烟酰胺的含量.     

Polymorphism, pseudopolymorphism, and amorphism of peracetylated alpha-, beta-, and gamma-cyclodextrins

Polymorphism, pseudopolymorphism, and amorphism of hexakis(2,3,6-tri-O-acetyl)-alpha-cyclodextrin (TAalphaCyD), heptakis(2,3,6-tri-O-acetyl)-beta-cyclodextrin (TAbetaCyD), and octakis(2,3,6-tri-O-acetyl)-gamma-cyclodextrin (TAgammaCyD) were investigated using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powder X-ray diffractometry (XRPD), Fourier transform infrared spectroscopy (FTIR) and optical microscopy. An anhydrous and a bi-hydrate crystalline forms of TAalphaCyD, two monotropic anhydrous polymorphs and three pseudopolymorphs (i.e. methanolate, hydrate, and isopropanolate-hydrate) of TAbetaCyD, as well as two monotropic anhydrous polymorphs and isostructural pseudopolymorphs (e.g. hydrate and isopropanolate-hydrate) of TAgammaCyD were isolated and characterized. The amorphous forms of each TACyD were also obtained. Thermal data for desolvation of TAalphaCyD.2H2O and TAbetaCyD.CH3OH were reconciled with their crystal packing features. Melting temperatures and enthalpies of the crystalline forms of each TACyD can be referred to for possible solid-state interactions with drugs.     

Alcohol,Age, and Piloting: Judgment,Mood, and Actual Performance

We have previously described acute and carry-over effects of alcohol on young and older pilots' performance. In the present paper we report the effects of alcohol and age on self-assessment of performance and mood in the same study. Young and older pilots flew in a simulator during an alcohol and placebo condition. In the alcohol condition, they flew after reaching. 04 g/dL (.04%) BAL, after. 10% BAL, and then 2,4, 8,24, and 48 h after. 10% BAL (they flew at the same times in the placebo condition). They rated confidence in ability to fly, mood, alertness, and intoxication before each flight, and perceived workload and performance after each flight. As reported in Morrow et al., alcohol had both acute and carry-over effects for 8 h on actual flight performance, with greater acute impairment for older pilots. The present study reports that these older pilots tended to be more aware than the young pilots of acute and carry-over alcohol impairment out to 4 h. By 8 h, however, all pilots were unaware of impairment. Alcohol also had a biphasic effect on mood, which increased on the ascending limb and decreased on the descending limb of the BAL curve.     

Lesbian,Gay, Bisexual,and Transgender Youth: Health Concerns,Services, and Care

Abstract

This paper was developed from a presentation made at the FDA/Industry Workshop held at Sandoz Research Institute, East Hanover, New Jersey on November 20, 1986.     

Smooth-pursuit eye movements,and diazepam,CPZ, and secobarbital

This study examined the effects on smooth-pursuit eye tracking of single doses of CPZ (0.667 and 1.334 mg/kg), diazepam (0.071, 0.142, and 0.284 mg/kg), and secobarbital (100 mg). Only the barbiturate significantly affected the ability to follow a moving target with smooth-pursuit eye movements. In repeated testing of a single subject, 130 mg of secobarbital disrupted smooth-pursuit movements at least until 24 hrs after ingestion.This study was supported in part by grant MH-19477, USPHS, and USFDA contract No. 72-42. Dr. Holzman is the recipient of Research Scientist Award No. K5-MH-70900, USPHS. We express our thanks to Dr. Alfred Heller for helpful comment.     

Temperature,pH, salinity,hardness, and particulates mediate nickel toxicity to eubacteria,an actinomycete,and yeasts in lake,simulated estuarine,and sea waters

The survival of some eubacteria, an actinomycete, and yeasts after acute and chronic exposures to nickel (Ni) in lake, simulated estuarine, and sea waters and the influence of environmental factors on Ni toxicity were determined. Nickel toxicity to microbes in marine systems was reduced by increasing the salinity, by decreasing the temperature, and by the incorporation of simulated sediment. The toxicity of Ni to microbes in fresh water was reduced by increasing the pH, by increasing the hardness, and by the incorporation of suspended particulates. Chronic toxicity studies indicated that fresh waters are more sensitive than marine waters to Ni pollution, as microbial survival was greater in marine than in fresh waters stressed with equivalent concentrations of Ni.     

Gradualism, identity, reinforcements, and change

This paper reflects the ongoing development of gradualism, a drug treatment perspective that seeks to make use of the full array of effective, creative, and innovative harm reduction and abstinence-oriented treatments available to help addicted individuals move along a continuum from active/chaotic use to abstinence or moderation, as appropriate. The essence of gradualism is an emphasis on positive change and transformation as therapeutic goals. The paper first looks at manifestations of gradualism in harm reduction treatment facilities. Following this is a discussion of the role of identity transformation in the change process. The final section explores how contingency management or motivational incentive interventions could be used in harm reduction settings to facilitate this kind of therapeutic movement.     

Opiates,catecholamines, behavior,and mood

Indirect evidence has linked opioid reinforcement with changes in noradrenergic metabolism secondary to drug administration. Methodological precedents for biobehavioral correlations in depressive illness have suggested an important association between changes in mood and biogenic amine excretion patterns in the urines of patients during depression and recovery. This paper presents preliminary data on the possible relationship between changes in catecholamine excretion that were observed and the changes in behavior, mood, psychiatric status, and cardiorespiratory physiology secondary to heroin administration and methadone-assisted withdrawal. This study focuses on the urinary excretion of MHPG, since an appreciable fraction of this metabolite is probably derived from norepinephrine originating in the brain. The subjective changes in mood associated with heroin use, the decrease in respiratory rate, and the behavioral and mental status effects associated with opiate intoxication were observed only in the individuals whose MHPG excretion increased during the period of opiate administration.