GC/MS法同时检测生物样品中苯丙胺、甲基苯丙胺及MDMA

目的:建立体液和组织中苯丙胺、甲基苯丙胺和3,4 -亚甲基二氧基甲基苯丙胺(MDMA)的简便快速、灵敏可靠的GC/MS检测方法。方法:样品经碱化,乙醚提取,TFA衍生化后,GC/MS全扫描定性检测,选择离子扫描(SIM)定量分析。结果:几种药物在血浆中的线性范围为0 .0 2 - 2 . 0 μg·ml-1,最低检出浓度为0 . 0 0 5 μg·ml-1(S/N≥3) ;肝脏中线性范围为0 . 0 5 - 5. 0 μg·g-1,最低检出浓度0. 0 .10 μg·g-1(S/N≥3)。相关系数大于或等于0 9980 ;回收率在92. 1% - 10 5. 2 %之间。结论:GC/MS方法适用于生物样品中苯丙胺、甲基苯丙胺和MDMA浓度的检测。     

干姜和白术挥发油提取工艺

目的研究干姜和白术挥发油的提取工艺。方法用共水回流冷凝法分别提取干姜和白术的混合挥发油、干姜挥发油以及白术挥发油 ,并将提取的挥发油经气相色谱 质谱 (GC MS)技术检测其主要成分。结果经GC MS分析 ,3种挥发油的主要成分一致 ,性质稳定。结论共水回流冷凝法对干姜和白术混合提取挥发油的工艺可行、简便 ,适合工业化生产     

北京地区零包毒品滥用形势分析

目的:对海洛因、甲基苯丙胺、氯胺酮三类零包毒品进行分析,了解该三类毒品各自在含量、价格方面的变化以及北京地区零包毒品流行的大概趋势,为禁毒部门提供参考信息。方法:收集北京地区2004-2009年毒品消费市场上最流行的三类零包毒品海洛因、甲基苯丙胺、氯胺酮,采用GC和GC/MS方法进行定性、定量分析。结果:三类毒品的价格比较稳定;甲基苯丙胺、氯胺酮的含量稳定,稀释剂使用较少;海洛因含量变化范围较大,且稀释剂种类繁多。结论:海洛因的滥用数量下降,甲基苯丙胺滥用呈上升趋势,氯胺酮的滥用较平稳;应加强对毒品稀释剂的管理。     

橄榄肉超临界CO2萃取物GC/MS分析

目的 分离鉴定橄榄肉成分.方法 采用超临界CO2萃取方法进行橄榄肉成分提取,提取物进行气相色谱/质谱联用(GC/MS)分析.结果 橄榄肉萃取物得率为7.39％,GC/MS共分离出67个组分,初步鉴定出36种成分,主要成分为十八碳-9-烯酸、麦角甾烷、3-甲基-3-乙基戊烷、9,12-十八碳二烯酸、n-十六酸等等,并应用...     

糖尿病合并非酒精性脂肪性肝病患者尿代谢组学研究

目的:运用气相色谱-质谱联用技术(GC/MS)技术观察糖尿病合并非酒精性脂肪性肝病(NAFLD)患者尿液中小分子代谢物,发现用于糖尿病合并NAFLD诊断的潜在生物标志物,为糖尿病合并NAFLD的发生机制和早期诊断提供代谢水平上的依据.方法:采用GC/MS检测20例正常人(正常组)、20例单纯糖尿病患者(单纯组)以及30...     

大蒜油的提取及其低温下稳定性研究

目的 :从昆明紫皮独头蒜中提取 -萃取大蒜油 ,并对其低温保存下稳定性进行考察。方法 :采用有机溶剂提取-萃取大蒜油 ;用气相色谱 /质谱法 (GC/ MS)鉴定大蒜油中主要成分 ;用 GC法观察低温保存下大蒜油有效成分的稳定性。结果 :大蒜的出油率为 0 .132 % ;其主要成分二烯丙基二硫醚、二烯丙基三硫醚各占 13.5 %、14 .8% ;前者在 3个月的监测期中各月含量分别为 13.4 7%、13.36 %及 13.89% ,后者含量分别为 14 .84 %、14 .90 %及 14 .2 7%。结论 :大蒜油的提取工艺简单 ,有效成分含量高 ,低温保存下稳定性好 ,可较长期保存。     

GC/MS在苯丙胺类药物分析中的应用

苯丙胺类药物的滥用已经成为世界严重的社会问题之一。在过去的几年中,大量的文章报道了血、尿及毛发中苯丙胺类药物的检测和鉴定。通过使用不同的检测器,最低检测浓度已经达到了ng·ml-1。这里我们主要介绍GC/MS在苯丙胺类药物分析中的应用以及还存在的一些不足之处。用于确定血、尿及毛发中苯丙胺类药物的大多数GC/MS程序,基本上都遵循下列原则:样品在经过液液提取(LLE)或固相提取(SPE)之后,随之进行衍生化,然后目标分析物在熔融的石英毛细管柱上被分离,并以选择离子检测(SIM)模式进行定量分析与检测,而且在大多数情况下,选择的内…     

UPLC-MS／MS法测定F351中催化剂四丁基溴化铵的残留量

目的:建立超高效液相色谱-质谱联用(UPLC—MS/MS)检测一类新药 F351原料药中催化剂四丁基溴化铵残留量的方法。方法:色谱柱为 Waters Atlantis HILIC Silica(2.1 mm×100 mm,3μm),流动相:乙腈-0.1 mol·L~(-1)甲酸铵溶液(pH=3.5)95:5,流速0.2 mL·min~(-1)。经石油醚和水(1:1)提取出的四丁基溴化铵通过 UPLC—MS/MS 进行检测。结果:本法的线性范围为5～100 ng·mL~(-1)(r=0.9996);最低检测限为2.9×10~(-12)g;回收率为97.1%。结论:本法操作简便,结果准确,可用于新药 F351对催化剂四丁基溴化铵的质量控制。     

白术超临界CO_2流体萃取部位脂溶性成分的GC/MS分析

目的:对白术超临界流体CO2提取物中脂溶性化学成分进行分析鉴定。方法:采用超临界CO2流体萃取技术从白术中提取挥发油;气相色谱-质谱法(GC/MS)分析鉴定脂溶性成分的化学成分,色谱柱为DB-5MS毛细管柱,载气为氦气,流速为2.0ml/min,柱温以10℃/min的升温速率从70℃升至250℃;质谱采用EI离子源。结果:共分离鉴定出19个色谱峰,大部分为不饱和脂肪酸类和酯类,占色谱总流出峰面积的96.2%。结论:可采用GC/MS法分析白术脂溶性部分的化学成分,以为白术的进一步开发和利用提供参考。     

GC／MS法检测头发中3，4-亚甲基二氧甲基安非他明

目的:建立了用GC/MS法检测吸毒嫌疑人头发中摇头丸主要成分3,4-亚甲基二氧甲基安非他明。方法:取头发约100 mg洗净、剪碎,以乙基吗啡为内标,0.1 mol·L-1盐酸水解,氯仿-异丙醇(3:2)混合溶剂提取。提取物经MSTFA衍生化后采用GC/MS分析。采用HP-1色谱柱(12 m×0.25 mm,0.33μm),柱温为100℃,保持2 min后以40℃·min-1升至260℃,继续以10℃·min-1升至280℃,保持2 min,载气为氦气(99.999％)。进样口温度为250℃,检测器温度为280℃,能量为70 eV。结果:3,4-亚甲基二氧甲基安非他明在1-75 ng·mg-1浓度范围内线性关系良好,相关系数0.998,回收率79.7％,日内误差RSD为6.5％,最低检测限为1 ng。结论:本法快速、可行,为获得关于长期药物滥用史的资料提供了一种检测技术。     

Intravenous self-injection of four novel phenethylamines in baboons

The present study evaluated the intravenous self-administration of four substituted phenethylamines, using a substitution procedure in baboons. Baboons were trained to self-inject 0.32mg/kg/injection cocaine under a fixed-ration (FR) schedule, with a 3h timeout following each injection. Doses of (+/-)-N-ethyl-3, 4-methylenedioxyamphetamine HCI (MDE), (+/-)-N-hydroxy-3, 4-methylendioxyamphetamine HCI (N-OH-MDA), (+)-N-N-dimethylamphetamine HCI (NNDMA), and 4-bromo-2,5-dimethyoxy-beta-phenethylamine (BDMPEA) and their vehicles were substituted for cocaine for 15 or more successive days. High doses of MDE and N-OH-MDA maintained self-injection; however, NNDMA and BDMPEA self-injection was less consistent. NNDMA did not reliably maintain self-injection, whereas one or more doses of BDMPEA maintained self-injection in each of three baboons. Intermediate to high doses of all four compounds decreased food pellet intake maintained under a FR schedule of reinforcement on a different lever. In some baboons, high doses of N-OH-MDA, NNDMA and BDMPEA produced signs of behavioral toxicity (e.g. cyclic pattern of self-injection, behavioral agitation, stereotypical movements) that were similar to those previously observed after administration of high doses of classic psychomotor stimulants such as d-amphetamine; however, the severity and profile of this behavioral toxicity differed between compounds. Thus, the present study documents both similarities and differences in the behavioral profiles of these four phenethylamines.     

Analysis of underivatized amphetamines and related phenethylamines with high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry

Amphetamine, methamphetamine, illicit designer phenethylamines (MDA, MDEA, MDMA, MBDB, and BDMPEA), and other phenethylamines (benzyl-1-phenylethylamine, cathinone, ephedrine, fenfluramine, norfenfluramine, phentermine, 1-phenylethylamine, phenylpropanolamine, and propylhexedrine) were extracted from serum using a solid-phase extraction procedure. The extracts were examined with high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS). The drugs were separated on ODS column in acetonitrile/50 mM ammonium formate buffer (pH 3.0) (25:75) as a mobile phase. Full-scan mass spectra of drugs examined by means of APCI with collision-induced dissociation showed protonated molecular ions and fragments typical for particular drugs. LC-APCI-MS allowed an unequivocal differentiation of all drugs involved. The quantitation was performed using selected ion monitoring of protonated molecular ions and fragments of drugs involved and their deuterated analogues. The limits of detection ranged from 1 to 5 microg/L serum, and the recoveries ranged from 58 to 96%. A linear response was observed for all drugs in the range from 5 to 500 microg/L. The method was applied for routine determination of amphetamine, MDMA, MDA, and MDEA in one run. Solid-phase extraction used assured simultaneous isolation of various groups of basic drugs of forensic interest (opiates, cocaines, phenethylamines, and benzodiazepines) from biofluids.     

Partition coefficients of low-molecular-weight volatile chemicals in various liquids and tissues

Partition coefficients are required for developing physiologically based pharmacokinetic models used to assess the uptake, distribution, tabolism, and elimination of volatile chemicals in mammals. A gas-phase vial equilibration technique is presented for determining the liquid:air and tissue:air partition coefficients for low-molecular-weight volatile chemicals. This technique was developed from two previously described medium:air methods, relied solely on measurement of chemical concentration in the gas phase, and, compared to earlier work, extends the range of chemicals and tissues examined. Partition coefficients were determined with 0.9% saline, olive oil, and blood, liver, muscle, and fat tissues from rats for 55 compounds. Human blood:air coefficients were determined for 36 compounds and several blood:air values were also determined in the mouse and for one compound in the hamster. An approach is described for predicting the tissue solubilities of untested compounds based on oil:air and saline:air coefficients using regression analyses. A similar approach is used to model fat:air coefficients in terms of oil:air values and to model human blood: air coefficients in terms of rat blood:air coefficients.     

慢性湿疹和皮炎126例不同患病部位斑贴试验结果分析

目的:探讨湿疹和皮炎等变态反应性疾病的接触性致敏原及其不同患病部位致敏原的特点。方法:应用"瑞敏牌"斑贴试剂盒检测126例慢性湿疹和皮炎患者接触性致敏原。结果:列前8位的常见致敏原分别是硫酸镍、芳香混合物、硫柳汞、重铬酸钾、对苯二胺、甲醛、对苯类、卡巴混合物;引起面部湿疹和皮炎的致敏原主要为芳香混合物、重铬酸钾、对苯二胺,手部主要为硫柳汞、芳香混合物、重铬酸钾、对苯二胺,躯干、四肢主要为硫酸镍和硫柳汞,脐周主要为硫酸镍。结论:斑贴试验有助于明确慢性湿疹和皮炎患者的接触性致敏原,并发现不同部位皮炎和湿疹常见致敏原的不同。     

PERMEABILITY OF THE DEVELOPING AND MATURE BLOOD-BRAIN BARRIERS TO THEOPHYLLINE IN RATS

1. In the present study, the uptake of theophylline and L-glucose into the adult and neonatal rat brain has been investigated. Steady state cerebrospinal fluid (CSF) and brain concentrations of theophylline were reached within 1 h following a single intraperitoneal (i.p.) injection, whereas steady state CSF and brain concentrations of L-glucose were not approached until after 5 h. 2. Steady state brain:plasma and CSF:plasma concentration ratios for theophylline and L-glucose in neonatal rats were significantly higher than ratios in adult rats. Erythrocyte:plasma ratios for theophylline in neonatal rats were also significantly higher than ratios in adult rats. Steady state ratios for theophylline were significantly higher than those for L-glucose in both neonatal and adult rats. 3. Respiratory acidosis (pH 6.9–7.0) did not affect steady state CSF:plasma or brain.-plasma ratios for theophylline in neonatal or adult rats. In contrast, steady state CSF:plasma and brain:plasma ratios for L-glucose were increased by respiratory acidosis. 4. The lower steady state CSF:plasma, brain:plasma and erythrocyte:plasma ratios for theophylline in adult rats are likely to be due to a higher concentration of plasma proteins in adult blood compared with neonates, with a greater retention of protein-bound (non-exchangeable) theophylline in adult blood, and are unlikely to be due to p-glycoprotein-mediated efflux of theophylline at the adult blood-brain barrier.     

Clinical evaluation of sustained release preparations of cefaclor in dental infections. Comparative double blind clinical studies of sustained release preparations with a regular preparation of cefaclor

In vitro viable cell count studies of sustained release preparations of cefaclor (CCL) conclude that the mixture of nonenteric and enteric coated granules of CCL in the ratio of 4 to 6 is the most appropriate form (4:6 form) for the sustained release preparation of CCL. In order to clinically confirm the above conclusion, comparative double blind clinical studies of 3 mixtures forms (2:8, 4:6 and 6:4 forms) with a regular preparation (CCL form) were conducted in dental infections regarding efficacy, safety, and usefulness of the 4 forms. Evaluable cases for efficacy and usefulness were 364 in total (96 cases for the 2:8 form group, 89 cases for the 4:6 form group, 89 cases for the 6:4 form group, and 90 cases for the CCL form group). Evaluable cases for safety were 404 cases in total (102 for the 2:8 form, 100 for the 4:6 form, 102 for the 6:4 form, and 100 for the CCL form). Daily dose of the 3 forms of sustained release preparations was 375 mg b.i.d. after breakfast and dinner and that of the CCL form 250 mg t.i.d. after breakfast, lunch and dinner. Following are the results of the clinical studies: There were no significant differences among the 4 patient-groups (2:8 form, 4:6 form, 6:4 form, and CCL form) regarding background factors of the patients and findings of their subjective and objective symptoms before the initiation of the administration, and it was therefore confirmed that there were no problems in conducting the comparative double blind clinical studies. Overall clinical effective rate determined by the efficacy evaluation criteria of the Japanese society of oral surgery (JSOS) were 89.5% at day 3 and 94.8% at day 5 in the 2:8 form group, 87.4% at day 3 and 95.5% at day 5 in the 4:6 form group, 86.4% at day 3 and 91.0% at day 5 in the 6:4 form group, and 93.3% at day 3 and 96.7% at day 5 in the CCL form group. The effective rate determined by the physicians who actually treated the patients were 84.4% in the 2:8 form group, 87.6% in the 4:6 form group, 84.1% in the 6:4 form group, and 87.8% in the CCL form group. In both judgments by the efficacy evaluation criteria of JSOS and the physicians, there were no significant differences among the 4 forms regarding overall clinical efficacy.(ABSTRACT TRUNCATED AT 400 WORDS)     

Effect of gender on the pharmacokinetics of ofloxacin

STUDY OBJECTIVES: To assess the influence of gender on the pharmacokinetics of ofloxacin. DESIGN: Open-label study. SETTING: Academic medical center. PATIENTS: Five healthy men and seven healthy women volunteers. INTERVENTIONS: Subjects received a single oral dose of ofloxacin 400 mg, and serial blood samples were collected for 24 hours. Plasma concentrations of ofloxacin were determined by high-performance liquid chromatography and pharmacokinetic parameters were determined. Statistical comparisons between genders were made with the Wilcoxon rank sum test. MEASUREMENTS AND MAIN RESULTS: Median volume of distribution at steady state/systemic bioavailability (V(ss)/F) was significantly smaller in women than in men, although when normalized for total body weight there were no differences. Except for terminal elimination half-life, which was 10% shorter in women, no other pharmacokinetic values were significantly different between genders. Median peak concentrations, although not statistically different, were 28% higher in women. CONCLUSION: Ofloxacin V(ss)/F values were smaller in women than in men, explained by gender-related differences in weight.     

An economic analysis of a randomized, controlled, multicenter study of clinical pharmacist interventions for high-risk veterans: the IMPROVE study. Impact of Managed Pharmaceutical Care Resource Utilization and Outcomes in Veterans Affairs Medical Centers

STUDY OBJECTIVE: To determine if clinical pharmacists could affect economic resource use and humanistic outcomes in an ambulatory, high-risk population. DESIGN: Prospective, randomized, controlled study. SETTING: Nine Veterans Affairs medical centers. PATIENTS: Patients who were at high risk for medication-related problems. INTERVENTION: Patients were randomized to usual medical care with input from a clinical pharmacist (intervention group) or just usual medical care (control group). MEASUREMENTS AND MAIN RESULTS: Of 1,054 patients enrolled, 523 were randomized to the intervention group and 531 to the control group. The number of clinic visits increased in the intervention group (p=0.003), but there was no difference in clinic costs. Mean increases in total health care costs were $1,020 for the intervention group and $1,313 for the control group (p=0.06). CONCLUSION: Including the cost of pharmacist interventions, overall health care expenditures were similar for patients randomized to see a clinical pharmacist versus usual medical care.     

Comparison of methods used for estimating pharmacist counseling behaviors.

OBJECTIVE: To compare the rates reported for provision of types of information conveyed by pharmacists among studies for which different methods of estimation were used and different dispensing situations were studied. DATA SOURCES: Empiric studies conducted in the US, reported from 1982 through 1992, were selected from International Pharmaceutical Abstracts, MEDLINE, and noncomputerized sources. STUDY SELECTION: Empiric studies were selected for review if they reported the provision of at least three types of counseling information. DATA EXTRACTION: Four components of methods used for estimating pharmacist counseling behaviors were extracted and summarized in a table: (1) sample type and area, (2) sampling unit, (3) sample size, and (4) data collection method. In addition, situations that were investigated in each study were compiled. DATA SYNTHESIS: Twelve studies met our inclusion criteria. Patients were interviewed via telephone in four studies and were surveyed via mail in two studies. Pharmacists were interviewed via telephone in one study and surveyed via mail in two studies. For three studies, researchers visited pharmacy sites for data collection using the shopper method or observation method. Studies with similar methods and situations provided similar results. CONCLUSIONS: Data collected by using patient surveys, pharmacist surveys, and observation methods can provide useful estimations of pharmacist counseling behaviors if researchers measure counseling for specific, well-defined dispensing situations.     

北京地区高学历吸毒者的情况分析

目的:了解北京地区高学历吸毒者的情况,为采取有效防范措施提供依据。方法:自拟调查问卷对北京市安康医院戒毒中心2000年1月1日-2003年12月31日收治的戒毒人员中大专以上高学历者进行逐项登记,并对吸毒原因、毒品滥用等情况分析。结果:高学历吸毒者共计431例,占同期戒毒的4.52%,其中男265例(61.48%),女166例(38.52%)。婚姻状况:未婚289例(67.05%),已婚100例(23.20%);职业:以无业为主,219例(50.81%),其次为职员,73例(16.94%);吸毒主要原因:好奇264例(61.25%)、受他人(朋友)影响112例(25.99%);主要滥用毒品的种类:海洛因274例(63.57%)、“摇头丸”130例(30.16%);滥用方式:海洛因滥用者中烫吸155例(57.57%)、注射119例(43.43%),“摇头丸”均为口服,其中119例(91.54%)兑于酒或饮料中使用;大麻均为烟吸,“K粉”均为兑于饮料中使用。有86.92%(113/130)的“摇头丸”滥用者认为服用摇头丸不会成瘾。结论:高学历吸毒人群以未婚、无固定职业为主体,高学历者好奇心强,易受他人影响,对新型毒品(摇头丸)知识欠缺,有关部门应加强宣传教育。