高效薄层色谱法检测尿中硝西泮的代谢物7-氨基硝西泮

目的 建立用高效薄层色谱法定性及半定量测定人尿中硝西泮的代谢物7-氨基硝西泮(7ANIZ)含量的方法。方法 人口服治疗量10 mg硝西泮后,在pH 9条件下用乙醚进行提取,分析物斑点用氟罗里丝进行荧光显色,紫外灯下(366nm)观察荧光斑点;根据斑点荧光显色情况及强度进行7ANIZ定性及半定量检测。结果 尿中硝西泮代谢物7ANIZ检出限为5 ng/ml,测量限为15 ng/ml。结论 人口服治疗量10 mg硝西泮,用高效薄层色谱法可定性及半定量测定48 h内排泄尿中的7ANIZ。     

A screening method for urinary methamphetamine--latex agglutination inhibition reaction test

Methamphetamine in urine samples from abusers was detected by the latex agglutination inhibition reaction test with latex-antibody (Latex-Ab) and latex-methamphetamine (Latex-MA) reagents. Anti-methamphetamine antibody was produced in rabbits by immunization with bovine serum albumin (BSA)-methamphetamine conjugate. Latex particles were coated with antibodies or with rabbit serum albumin (RSA)-methamphetamine conjugate to obtain Latex-Ab and Latex-MA reagents, respectively. The results are read at 4-5 min after mixing the latex reagents. The sensitivity of this method for methamphetamine was 0.4 micrograms/ml urine. Methamphetamine analogs (methylephedrine, amphetamine, phentermine, methoxyphenamine, ephedrine, beta-phenylethylamine, OH-methamphetamine, OH-amphetamine, and OH-ephedrine) all cross-react in varying degrees, while glucosiurea and albuminurea give false positive results in the tests. Though attention must be paid to these effects this simple and rapid test is suitable for the mass screening of urine samples.     

Simultaneous analysis of six amphetamines and analogues in hair, blood and urine by LC-ESI-MS/MS: Application to the determination of MDMA after low Ecstasy intake

A rapid and sensitive method using LC-MS/MS triple stage quadrupole for the determination of traces of amphetamine (AP), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA, “ecstasy”), 3,4-methylenedioxyethamphetamine (MDEA), and N-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine (MBDB) in hair, blood and urine has been developed and validated. Chromatography was carried out on an Uptisphere ODB C₁₈ 5 μm, 2.1 mm × 150 mm column (Interchim, France) with a gradient of acetonitrile and formate 2 mM pH 3.0 buffer. Urine and blood were extracted with Toxitube A^® (Varian, France). Segmented scalp hair was treated by incubation 15 min at 80 °C in NaOH 1 M before liquid–liquid extraction with hexane/ethyl acetate (2/1, v/v). The limits of quantification (LOQ) in blood and urine were at 0.1 ng/mL for all analytes. In hair, LOQ was <5 pg/mg for MA, MDMA, MDEA and MBDB, at 14.7 pg/mg for AP and 15.7 pg/mg for MDA. Calibration curves were linear in the range 0.1–50 ng/mL in blood and urine; in the range 5–500 pg/mg for MA, MDMA, MDEA and MBDB, and 20–500 pg/mg for AP and MDA. Inter-day precisions were <13% for all analytes in all matrices. Accuracy was <20% in blood and urine at 1 and 50 ng/mL and <10% in hair at 20 and 250 pg/mg. This method was applied to the determination of MDMA in a forensic case of single administration of ecstasy to a 16-year-old female without her knowledge during a party. She suffered from hyperactivity, sweating and agitation. A first sample of urine was collected a few hours after (T + 12 h) and tested positive to amphetamines by immunoassay by a clinical laboratory. Blood and urine were sampled for forensic purposes at day 8 (D + 8) and scalp hair at day 60 (D + 60). No MDMA was detected in blood, but urine and hair were tested positive, respectively at 0.42 ng/mL and at 22 pg/mg in hair only in the segment corresponding to the period of the offence, while no MDA was detectable. This method allows the detection of MDMA up to 8 days in urine after single intake.     

Successful DNA typing of ultrafiltered urines used to detect EPO doping

Endogenous and exogenous erythropoietin (EPO) present in urine can be distinguished according to their isoelectric profiles. This methodology requires urine samples to be concentrated about 200 to 1000 times with manipulations that should remove most of the cells occurring in the original sample. In this study, we tried to obtain DNA profiles from 10 ultrafiltered urines (retentates) in order to evaluate whether a formal genetic identification was technically feasible. No nuclear DNA profiles could be established from retentates, despite 34 PCR-cycles amplifications. Contrastingly, mitochondrial DNA (mtDNA) profiles were obtained for 9 out of the 10 retentates. Apart from some particularities, retentate mtDNA profiles were all distinct and matched mtDNA profiles of corresponding reference samples.     

尿中异丙嗪及其代谢物含量硅藻土萃取紫外导数光谱测定法

目的建立尿中异丙嗪原体及其代谢物异丙嗪亚砜的提取测定方法。方法取尿直接倒入硅藻土柱中，用二氯甲烷洗脱，收集洗脱液50℃水浴挥干。剩余物用3．0ml 0．05mol／L硫酸溶解。加入锌粉沸水浴加热，放冷，测定二阶导数光谱。结果异丙嗪亚砜和异丙嗪萃取率均达90％以上，线性范围0．5～5．0μg／ml。结论该方法操作简便，提取率高，重现性好，结果可靠。     

用双抗夹心间接ELISA方法检测p30确证人类精斑

检测p30确证精斑有下列几种方法:免疫扩散,免疫电泳,交叉免疫电泳,胶乳凝集抑制试验,薄层免疫分析和酶联免疫吸附试验(ELISA).这些方法各有优缺点,就灵敏度而论,则以     

养肝益水颗粒对高血压早期肾损害尿微量蛋白的影响

目的:观察养肝益水颗粒对高血压早期肾损害患者尿清蛋白排泄率(urinary albumin ex-cretion ratio,UAER)、尿微量清蛋白(microalbuminuria,MA)、β2微球蛋白(β2-microglobulin,β2-MG)、α1微球蛋白(α1-microglobulin,α1-MG)、转铁蛋白(transferrin,TRF),免疫球蛋白G(immu-noglobulin G,IgGu)的影响.方法:选择80例符合中医辨证的高血压早期肾损害患者,随机分为治疗组和对照组.两组均给予常规降压治疗.治疗组同时加服养肝益水颗粒.两组疗程均为4周.分别于治疗前和治疗4周后进行UAER、MA、α1-MG、β2-MG、TRF、IgGu测定.结果:治疗后两组UAER、MA、α1-MG、β2MG、TRF、IgGu水平均显著下降,且治疗组与对照纽比较,上述指标的差异具有显著性(P＜0.05,P＜0.01).结论:养肝益水颗粒具有减少高血压早期肾损害尿微量蛋白排出的作用.     

A high selective screening test for methamphetamine in human urine

A high selective screening test (Ad-Tip method) for methamphetamine in human urine has been devised. The method involves a brief extraction from a urine sample with an Ad-Tip (ODS-silica minicolumn), washing, eluting with modified Simon's reagent, and coloration with carbonate buffer. Detection limit of methamphetamine in urine is 1 microgram/ml and the test takes within 3 min/sample. The results of the Ad-Tip method were almost identical to those of laboratory analyses.     

一种制备酶标记抗体的新技术及在血痕种属鉴定的应用

本实验建立了一种过碘酸钠氧化法为基础、制备ＨＲＰ标记的免抗人ＩｇＧ抗体的新技术。首先以己二酰二肼作为肼化剂，在ＩｇＧ分子上接上肼基，然后以过碘酸钠作为氧化剂，使ＨＲＰ分子上的糖基氧化为醛基，进而使醛基与联结在ＩｇＧ分子上的肼基形成Ｓｃｉｆｆ氏碱而达到酶与抗体的联接。在用斑点ＥＬＩＳＡ方法鉴别血痕种属的研究中，该法制各的酶标记抗体具有高效价，高敏感度，高特异性等优点。