正交试验法优选血康胶囊提取工艺

目的：研究血康胶囊提取工艺。方法：采用正交试验法进行优选，以TLCS法测定人参皂苷Rg1的含量。结果：提取交数、乙醇浓度对人参皂苷Rg1提取率及干膏率有显性影响。结论：最佳提取工艺为500ml／L乙醇回汉提取2次，溶剂用量依次为6，5倍，提取时间为1．5，1．5h。     

Simultaneous quantification of opiates, cocaine and cannabinoids in hair

The present paper describes a sensitive method developed in our laboratory for the simultaneous analysis of opiates (morphine, codeine and monoacetylmorphine), cocainics (cocaine and benzoylecgonine) and cannabinoids (Δ⁹-tetrahydrocannabinol and 11-nor-Δ⁹-tetrahydrocannabinol-9-carboxylic acid) in hair samples. After decontaminating the sample with dichloromethane, two consecutive hydrolyses were performed in order to achieve the best conditions for extracting the three kinds of drugs from the protein matrix. First the opiate and cocainic compounds were extracted by means of a soft acidic hydrolysis with 0.1 N HCl at 50 °C overnight and organic solvent extraction at pH 9.2. The cannabinoids need a stronger basic hydrolysis with 11.8 N KOH for 10 min at laboratory temperature. After adding maleic acid, the cannabinoids were extracted with an organic solvent. The derivatization was carried out with heptafluorobutyric anhydride and hexafluoropropanol. Calibration curves were linear between 0.5–100 ng/mg of hair. Recovery and reproducibility were assured. The quantification limits ranged between 0.04–0.26 ng/mg of hair. Seventy hair samples from known drug abusers were cut into 1-cm segments and analyzed by this method. The ranges of measured concentrations (ng/mg) were 0.31–89 for cocaine, 0.1–5.76 for benzoylecgonine, 0.34–45.79 for morphine, 0.45–39.59 for codeine, 0.09–48.18 for monoacetylmorphine, 0.06–7.63 for THC and 0.06–3.87 for THC---COOH. The results of sectional analyses agreed with the self reported drug histories. The usefulness of this method is in assessing earlier drug consumption, and also at the same time obtaining a chronological profile of the consumption of these three types of drugs.     

Phenobarbital in hair and drug monitoring

Phenobarbital analysis was performed in vertex hair of patients by gas chromatography mass spectrometry (GC/MS). After washing with dichloromethane, about 250 mg were ground to dust in a ball mill. A 50-mg sample was stirred mechanically for 10 min with 3 ml of NH₄Cl/HCl buffer (pH 2.0) containing phenobarbital D₅. A solid phase extraction was performed (extrelut Merck) and elution was achieved with chloroform/isopropanol/n-heptane (50:17:33; v/v). A full scan (40–240 uma) acquisition was realized by GC/MS with an ion trap (ITD 700 Finnigan) using a DB5-MS chromatographic column. Quantification was achieved by integrating dominants ions (phenobarbital, 204; phenobarbital D₅, 209). Compared to serum, hair concentrates phenobarbital during anti-epileptic therapy (average value 36.4 ng/mg, n = 40 vs. 18.7 mg/l, n = 23). A group correlation exists between phenobarbital in hair and phenobarbital in serum, and between phenobarbital in hair and clinic observation in some typical cases. Phenobarbital in hair yields good information over a long period, especially when blood collection has not been made, when clinical disorders are observed on long-term therapeutic observance.     

固相萃取技术分析生物检材中的鸦片成份

建立用国产GDX－403固相柱、GC／NPD毛细管气相色谱法，提取、净化生物检材中鸦片的方法。在1ml全血中添加1～4μg混合药物，回收率为79.2％～89.3％，RSD为2．61％～7．50％；在2g肝中添加2．5～10μg混合药物，回收率为72．9％～86．9％，RSD为2．27％～9．20％。该法回收率高，可用于检测人体内的微量鸦片成份。     

基于HTML结构的Web文本主题挖掘研究

随着数据挖掘应用的深入,非结构化和半结构化数据的挖掘,将成为下一个数据挖掘应用的热点。文本挖掘是一种典型的非结构化数据挖掘,而Web挖掘则是典型的半结构化数据挖掘。所以将信息处理技术中的汉语分词、信息抽取、语义分析等技术应用到Web挖掘研究技术发展的必然趋势。本文应对Web挖掘的特点,将运用数据抽取进行数据结构转换并把语义分析技术应用到数据抽取的过程中的思想,使数据提取更加准确。     

双溶剂提取法的优化

目的建立一种稳定的双溶剂提取圆珠笔油墨的实验体系,达到相对准确判断圆珠笔字迹书写时间的目的。方法依次用弱溶剂(氯苯)、强溶剂(N-N二甲基甲酰胺)溶解提取纸张上的圆珠笔油墨,点样在硅胶板上,薄层扫描得到吸收峰高值,而后根据吸收峰高值测算其相对提取率和标准偏差。结果找到了弱溶剂量10μl、取样量10~15片、弱溶剂溶解时间60s以及强溶剂量10μl的最佳实验条件。结论优化了双溶剂提取法,提高了该方法在检验鉴定中的准确度和可靠性。     

Testing human hair for drugs of abuse. IV. Environmental cocaine contamination and washing effects

Active cocaine use results in sequestration of parent drug in hair. In addition, hair has unique physicochemical properties that permit absorption of cocaine from the environment. When hair is tested for evidence of cocaine, it is important to consider whether the positive test resulted from active drug use or environmental contamination. In a series of laboratory experiments, it was found that exposure of ‘cut’ hair to cocaine vapor (‘crack’ smoke) and to aqueous solutions of cocaine hydrochloride resulted in significant contamination of hair samples. Similar results were obtained with two subjects who were exposed to cocaine vapor in an unventilated room. The amount of contamination adsorbed by hair depended upon both time and extent of exposure. Washing the hair samples with methanol removed >70% of the cocaine contaminant after cocaine vapor exposure, but was less effective (<50%) following contamination with aqueous cocaine. Shampoo treatment cycles (overnight soaking) progressively removed increasing amounts of cocaine from the contaminated hair, but residual cocaine remained after 10 cycles. Studies were also performed to determine the usefulness of benzoylecgonine as a marker of active cocaine administration. Small amounts of benzoylecgonine (ca. 1 ng/mg) were formed in hair as a result of environmental contamination with cocaine. Also, it was found that benzoylecgonine could be adsorbed from illicit cocaine contaminated with benzoylecgonine. It was concluded that positive hair test results should be interpreted cautiously due to the possibility of environmental contamination from cocaine and related constituents.     

芦根中甾体的GC-TOFMS鉴定

目的：提取并测定芦根中甾族化合物的成分和相对含量。方法：采用气相色谱．飞行时间质谱法进行测定分析。结果：芦根提取物中含有4种甾体化合物。结论：该鉴定方法对药物成分的结构分析和临床用药具有指导意义。     

牙齿的DNA提取及STR分型研究

目的建立有效的牙齿DNA提取方法。方法使用物理及化学方法去除牙齿表面污染物,经脱钙、裂解、纯化从牙粉中提取DNA进行STR分型。结果对96例牙齿检材进行DNA检验,获得STR分型的有94例,在查找尸源的案件中发挥了重要作用。结论本方法操作简单快速,能够显著提高牙齿DNA检验的成功率。     

不同前处理方法提取牙齿DNA的比较

目的对三种不同前处理方法提取的牙齿DNA浓度进行比较,建立一种操作简便、经济适用、浓度较高的牙齿DNA提取的前处理方法。方法选择源自7具尸体的共21颗磨牙,每具尸体的3颗磨牙随机按牙屑法、球磨法、液氮研磨法进行前处理,并分别称取50 mg,采用Auto Mate Express~(TM)法医DNA提取系统提取DNA,对三种方法提取的DNA浓度和STR分型结果进行比较。结果牙屑法、球磨法和液氮研磨法提取的DNA质量浓度分别为0.055 6~1.989 1、0.036 6~1.175 6和0.037 8~1.249 0 ng/μL,牙屑法提取的DNA质量浓度较高(P0.05),且STR分型成功率高。结论牙屑法结合Auto Mate Express~(TM)法医DNA提取系统是提取牙齿DNA的一种切实可行的方法,可应用于法医学鉴定实践中。