北京市城市河流中精神活性物质的污染水平及环境风险

为评价北京市城市河流地表水体中5种精神活性物质〔METH(甲基苯丙胺)、AMP(苯丙胺)、KET(氯胺酮)、EPH(麻黄碱)和HA(羟亚胺)〕的环境风险,通过对固相萃取柱(Oasis HLB、Oasis MCX、Oasis WAX和Oasis PRiME HLB)类型、水样酸化、洗脱剂类型及体积等条件的确定,建立了同时测定水环境中精神活性物质的固相萃取-液相色谱-质谱(SPE-LC-MS/MS)联用方法,并对北京市城市河流地表水体中5种精神活性物质的质量浓度水平进行了调查,采用RQ(风险熵)法进行了风险评价. 结果表明,在水样未酸化条件下,Oasis MCX柱对精神活性物质的回收率最高,使用含5%(V/V)氨水的甲醇作为洗脱液,5种精神活性物质的回收率可以达到81.8%~91.1%. 地表水水体基质加标结果表明,5种精神活性物质的加标回收率均大于75.5%,相对标准偏差均小于10.0%. 方法检出限为0.30~0.80 ng/L,定量限为1.00~2.68 ng/L. 北京市7条城市河流中5种精神活性物质的质量浓度在1.00~99.51 ng/L之间. EPH在所有采样点均被检出且质量浓度较高,ρ(EPH)平均值为22.79 ng/L;ρ(AMP)相对较低,在1.54~11.23 ng/L之间,但AMP检出率为97.06%;ρ(METH)较高,平均值为14.63 ng/L,最高值(99.51 ng/L)出现在坝河. 研究显示,北京市地表水中5种精神活性物质的RQ均小于0.1,表明其可能的环境风险较低,但由于精神活性物质本身具有生物活性,它们对城市河流水生生态系统产生的潜在危害不容忽视.      

粉葛根腐病菌的生物学特性及防治研究

粉葛根腐病是粉葛生产上新发现的一种毁灭性土传病害。作者对病原作了人工分离和接菌试验，观测了温度、pH对病原菌菌丝体生长的影响；对防治药剂进行了筛选和试验，探讨了该病的有效防治药物及对策。     

成瘾者头发样品中滥用药物的GC—MS鉴定

本文采用气相色谱－质谱方法分离、鉴定成瘾者头发样品中的滥用药物，样品处理方法简单，甲醇一次超声提取，提取效果较好，样品用量少，仅需２０ｍｇ。应用该法对几例成瘾者头发样品进行了分析鉴定，不公检出几种代谢产物，而且检出药物的原形。     

双氯芬酸和醋氨酚对稀有鮈鲫早期生活阶段的毒性效应

随着非甾体抗炎药（NSAIDs）的持续使用与排放,世界各地的地表水、海水、地下水、污水厂进出水中均已频繁检测到该类药物,这对生态系统中各种非靶标生物造成了一定威胁.本研究评价了两种典型的非甾体抗炎药-双氯芬酸（Diclofenac）和醋氨酚（Acetaminophen）对中国特有物种稀有鮈鲫（Gobiocypris rarus）早期生活阶段的毒性效应.实验结果显示,醋氨酚的毒性较弱,当浓度达到48.4 mg·L^-1（NOEC）时,稀有鮈鲫的孵化率、死亡率、异常率、全长和干重均未表现出明显的中毒症状;而双氯酚酸的毒性则较强,当浓度达17.8 mg·L^-1（LC₁₀）时,即可导致稀有鮈鲫孵化率下降,当浓度达到10.2 mg·L^-1（LOEC）时,即可造成幼鱼外观和行为的显著异常,表明双氯芬酸对稀有鮈鲫的孵化和生长均产生了一定的致毒效应.同时,根据稀有鮈鲫和几种常用模式生物之间的孵化率、孵化后存活率、体长和双氯芬酸敏感性的比较结果,可认为稀有鮈鲫适用于污染物对鱼类早期生活阶段毒性效应的评估.     

在线固相萃取-液相色谱串联质谱法测定污水厂尾水中6种酸性药物

建立了大体积在线固相萃取-液相色谱串联质谱（Online-SPE-LC-MS）检测污水厂尾水中6种酸性药物的方法。10 mL水样采用0.45 μm微孔滤膜过滤后经自动进样器直接在线上样,经Atlantis T3柱（100 mm×4.6 mm×3 μm）富集,Atlantis T3柱（100 mm×2.1 mm×2.6 μm）色谱分离,ESI-/ESI+源同步切换扫描,多反应监测（MRM）模式对布洛芬、酮洛芬、双氯芬酸钠、吲哚美辛、苯扎贝特、卡马西平进行同时定量分析。基于外标法和标准加入法进行分析以消除基质效应。结果显示,6种酸性药物在0.1~200 ng/L范围内线性相关性较好（r≥0.996 4）,检出限（LOD）为0.01~0.16 ng/L,定量限（LOQ）为0.02~0.52 ng/L,加标回收率为94.3%~102%,相对标准偏差（RSD）为0.49%~10.1%。该法采用10 mL大体积进样,前处理简单、快速且重现性好,可有效实现污水厂尾水中6种酸性药物的定量分析。     

Design,synthesis, antinociceptive,and anti-inflammatory properties of thiazolopyrimidine derivatives

Ten 2-(substituted benzylidene)-7-(4-chlorophenyl)-5-(furan-2-yl)-2H-thiazolo[3,2-a]pyrimidin-3(7H)-one derivatives were synthesized and evaluated. A series of heterocyclic, 2-(substituted benzylidene)-7-(4-chlorophenyl)-5-(furan-2-yl)-2H-thiazolo[3,2-a]pyrimidin-3(7H)-one were synthesized by reaction of 7-(4-chloro phenyl)-5-(furan-2-yl)-2H-thiazolo[3,2-a]pyrimidin-3(7H)-one with appropriately substituted aldehydes in the presence of anhydrous sodium acetate and glacial acetic acid. The antinociceptive activity was evaluated by tail-flick technique, anti-inflammatory activity was evaluated by carrageenan-induced paw edema test and their ulcerogenicity index was determined. The para-substituted methyl, hydroxy, fluoro, chloro, bromo, and nitro derivatives showed significant antinociceptive and anti-inflammatory activities. The detailed synthesis, spectroscopic data, and pharmacological screening of the synthesized compounds were reported.     

Metabolism of aceclofenac in cattle to vulture‐killing diclofenac

The nonsteroidal anti‐inflammatory drug (NSAID) diclofenac is highly toxic to Gyps vultures, and its recent widespread use in South Asia caused catastrophic declines in at least 3 scavenging raptors. The manufacture of veterinary formulations of diclofenac has since been banned across the region with mixed success. However, at least 12 other NSAIDs are available for veterinary use in South Asia. Aceclofenac is one of these compounds, and it is known to metabolize into diclofenac in some mammal species. The metabolic pathway of aceclofenac in cattle, the primary food of vultures in South Asia, is unknown. We gave 6 cattle the recommended dose of aceclofenac (2 mg/kg), collected blood thereafter at intervals for up to 12 h, and used liquid chromatography with mass spectrometry in a pharmacokinetic analysis of aceclofenac and diclofenac in the plasma. Nearly all the aceclofenac administered to the cattle was very rapidly metabolized into diclofenac. At 2 h, half the aceclofenac had been converted into diclofenac, and at 12 h four‐fifths of the aceclofenac had been converted into diclofenac. Therefore, administering aceclofenac to livestock poses the same risk to vultures as administering diclofenac to livestock. This, coupled with the risk that aceclofenac may replace diclofenac in the veterinary market, points to the need for an immediate ban on all aceclofenac formulations that can be used to treat livestock. Without such a ban, the recovery of vultures across South Asia will not be successful.     

Development of an enzyme linked immunosorbent assay for the determination of phenothiazine drugs in meat and animal feeds

In this study, 2-chlorophenothiazine was used to synthesize a hapten for production of monoclonal antibody. The obtained monoclonal antibody showed high crossreactivities to chlorpromazine, promethazine and perphenazine, and showed low crossreactivities to acepromazine and fluphenazine. After evaluation of three coating antigens, a heterologous competitive indirect enzyme linked immunosorbent assay was developed to determine the five phenothiazines in animal feeds and the residues of chlorpromazine, promethazine and perphenazine in meat. The crossreactivities to the five analytes were in a range of 2.4%–98%. The limits of detection for the five drugs in feeds were in a range of 0.1–3.0 μg g^?1, and that for chlorpromazine, promethazine and perphenazine in meat were in a range of 0.5–0.8 ng g^?1. Their recoveries from standards fortified blank samples (chicken, pork and feeds) were in a range of 74.1%–96.5% with coefficients of variation of 6.4%–15.1%. Therefore, this method could be used as a rapid screen tool to determine phenothiazine drugs in animal feeds and animal derived foods.     

污水中常见违禁药物分析方法优化及验证

违禁药物作为一种新型污染物得到了环境科学界的广泛关注.本文根据国内外已有研究,比较了污水样的前处理条件如SPE柱和水样pH值、冲洗、酸化及复溶过程.结果表明,对实际污水样的前处理应将样品pH值调为2,选用Oasis MCX柱,无需除杂质的冲洗和氮吹过程的酸化步骤,因两种上机测定方法 HILIC-UPLC-MS/MS和C18-UPLC-MS/MS不同而分别选择200μL乙腈和100μL乙腈+100μL 5 mmol·L~(-1)乙酸铵复溶.通过比较HILIC法和C18法的保留时间及检出限、定量限、回收率和基质效应等方法评价指标,确定污水样的测定应选用C18-UPLC-MS/MS.最后,将优化后的测定方法用于分析北京市12家污水处理厂的进、出水样,验证了方法的可靠性,为违禁药物的污水流行病学研究和环境风险评价奠定了基础.