Simultaneous quantification of several classes of antibiotics in water,sediments, and fish muscles by liquid chromatography-tandem mass spectrometry

Precise and sensitive methods for the simultaneous determination of different classes of antibiotics, including sulphonamides, fluoroquinolones, macrolides, tetracyclines, and trimethoprim in surface water, sediments, and fish muscles were developed. In water samples, drugs were extracted with solid-phase extraction （SPE） by passing 1000 mL of water through hydrophilic lipophilic balanced （HLB） SPE cartridges. Sediment samples were solvent-extracted, followed by tandem SPE （strong anion exchange （SAX） ＋ HLB） clean-ups. Fish muscles were extracted by a mixture of acetonitrile and citric buffer （80：20, v/v） solution, and cleaned by SPE. Liquid chromatography-tandem mass spectrometry （LC-MS/ MS） with multiple reaction monitoring （MRM） detection was employed to quantify all compounds. The recoveries for the antibiotics in the spiked water, sediment, and fish samples were 60.2%-95.8%, 48.1%-105.3%, and 59.8%- 103.4%, respectively. The methods were applied to samples taken from Dianchi Lake, China. It showed that concentrations of the detected antibiotics ranged from limits of quantification （LOQ） to 713.6 ng- L1 （ofloxacin） in surface water and from less than LOQ to 344.8 μg·kg-1 （sulphamethoxazole） in sediments. The number of detected antibiotics and the overall antibiotic concentrations were higher in the urban area than the rural area, indicating the probable role of livestock and human activities as important sources of antibiotic contamination. In fish muscles, the concentration of norfioxacin was the highest （up to 38.5 μg·kg-1）, but tetracyclines and macrolides were relatively low. Results showed that the methods were rapid and sensitive, and capable of determining several classes of antibiotics from each of the water, sediment, and fish matrices in a single run.     

Simultaneous quantification of several classes of antibiotics in water,sediments, and fish muscles by liquid chromatography–tandem mass spectrometry

Precise and sensitive methods for the simultaneous determination of different classes of antibiotics, including sulphonamides, fluoroquinolones, macrolides, tetracyclines, and trimethoprim in surface water, sediments, and fish muscles were developed. In water samples, drugs were extracted with solid-phase extraction (SPE) by passing 1000 mL of water through hydrophilic lipophilic balanced (HLB) SPE cartridges. Sediment samples were solvent-extracted, followed by tandem SPE (strong anion exchange (SAX) + HLB) clean-ups. Fish muscles were extracted by a mixture of acetonitrile and citric buffer (80:20, v/v) solution, and cleaned by SPE. Liquid chromatography–tandem mass spectrometry (LC-MS/MS) with multiple reaction monitoring (MRM) detection was employed to quantify all compounds. The recoveries for the antibiotics in the spiked water, sediment, and fish samples were 60.2%–95.8%, 48.1%–105.3%, and 59.8%–103.4%, respectively. The methods were applied to samples taken from Dianchi Lake, China. It showed that concentrations of the detected antibiotics ranged from limits of quantification (LOQ) to 713.6 ng·L^-1 (ofloxacin) in surface water and from less than LOQ to 344.8 μg·kg^-1 (sulphamethoxazole) in sediments. The number of detected antibiotics and the overall antibiotic concentrations were higher in the urban area than the rural area, indicating the probable role of livestock and human activities as important sources of antibiotic contamination. In fish muscles, the concentration of norfloxacin was the highest (up to 38.5 μg·kg^-1), but tetracyclines and macrolides were relatively low. Results showed that the methods were rapid and sensitive, and capable of determining several classes of antibiotics from each of the water, sediment, and fish matrices in a single run.     

全自动固相萃取-超高效液相色谱串联质谱法测定地表水中18种头孢菌素

建立了超高效液相色谱串联质谱（UPLC-MS/MS） 法测定地表水中18种头孢菌素的方法。采用全自动固相萃取技术进行前处理,地表水样经HLB固相萃取小柱富集后,用10%（V/V）的甲酸溶液（溶剂为甲醇）洗脱。优选BEH Shield RP18（1.7μm,2.1mm×100mm） 色谱柱进行分离,在电喷雾正离子（ESI+）模式下电离,多反应模式（MRM）下检测,外标法定量。结果表明：18种头孢菌素在5.0～100 μg/L 范围内线性关系良好,相关系数（r）均＞0.999,方法检出限为0.5～1.8 ng/L,测定下限为2.0～7.2 ng/L。对地表水样品进行加标回收实验,18种头孢菌素的相对标准偏差（RSD）为0.5%～14.5%,加标回收率为64.3%～92.8%。该方法自动化程度高,结果稳定可靠,适用于地表水中头孢菌素的测定。     

CRISPR/Cas系统抵御细菌耐药

近年来,细菌耐药性问题在全球范围内日益严重,世界各地不断出现各种新型耐药基因及"超级细菌",以此形成的细菌耐药性污染已成为威胁全球公共卫生与环境安全的重大问题。目前除了在管理上规范合理用药和限制抗生素排放,应探讨抵御细菌耐药的分子机制,有效地从根本上遏制细菌耐药的产生。CRISPR系统作为一种天然免疫系统,可用来对抗入侵的外源性遗传物质,其结构和功能与细菌耐药及毒力因素密切相关,深入分析两者的关系有助于更好地理解细菌耐药机制,为防治细菌耐药提供了新的方向。     

地表水中抗生素复合残留对水生生物的毒性及其生态风险评价

针对上海地区地表水中混合并持久残留的抗生素对水生态的危害,测试了3种主要被使用的抗生素(磺胺甲恶唑,SMZ;土霉素,OTC;氟苯尼考,FF)对4个不同营养级的水生生物代表种(蛋白核小球藻、费氏弧菌、大型蚤和斑马鱼胚胎)的单一毒性和联合毒性,并进一步对生态风险进行评估来探究抗生素对水生态系统的综合作用。研究表明:水生生物对单一抗生素暴露的毒性敏感顺序为:蛋白核小球藻斑马鱼胚胎费氏弧菌大型蚤。用联合指数(CI)来评价抗生素二元混合物之间的相互作用时发现对于不同水生模式生物,抗生素之间的相互作用方式以拮抗作用(CI1)为主。通过与浓度加和(CA)和独立作用(IA)2个传统模型的预测效果比较,发现CI模型能准确预测到抗生素联合毒性偏离相加作用。由于养殖废水中这3种抗生素的含量均远高于其他水体(如黄浦江、长江口、工厂废水),其对不同营养级的水生生物均表现出较高的风险性,需要对养殖废水采取相应的风险削减措施;相比之下,其他水体中抗生素对费氏弧菌、斑马鱼胚胎、大型蚤均表现出低风险,但是对蛋白核小球藻仍具有一定的风险性,需要警惕抗生素对水体初级生产者的风险性。     

The need for growth promoting compounds in poultry meat production

Modern strains of broiler chicken are capable of achieving a 2.4 kg liveweight at 42d of age. This extremely fast growth is accomplished in part by balanced diets containing pharmaceutical growth promoting compounds. Over the last few years, a number of ethical questions have arisen regarding the use of such compounds. Such fast growth rate is accompanied by reduced bird welfare related to morbidity and mortality of a proportion of the birds. In two trials we have shown that acceptable growth rate can be achieved in diets without these compounds, and that economics of production are not adversely affected. It is concluded that future management programs for broiler chickens should consider a tempering of growth rate and that this could lead to improved bird well-being.     

两种常用兽药对作物发芽的生态毒性效应

采用室内生长箱培养的试验方法,研究了2种常用兽药磺胺嘧啶钠、环丙沙星对小麦、白菜和番茄种子发芽、根伸长、芽伸长的影响,分析了兽药和作物生长之间的剂量.效应关系,比较分析了小麦,白菜和番茄对2种兽药胁迫的敏感性.结果表明,根长抑制率和芽长抑制率与兽药浓度显著相关(p<0.05);种子发芽抑制率与2种兽药浓度不相关(p>0.05).2种兽药对根伸长和芽伸长的抑制明显强于对种子发芽的抑制.3种作物对磺胺嘧啶钠胁迫的敏感性依次为小麦＞白菜＞番茄;对环丙沙星胁迫的敏感性依次为白菜＞番茄＞小麦;磺胺嘧啶钠对3种作物的毒性效应明显强于环丙沙星.     

Sulfamethoxazole removal from polluted water by immobilized photocatalysis

The photocatalytic activity of TiO₂ deposits (Degussa P25 and Millennium PC500) has been studied using sulfamethoxazole (SMX) as a model water pollutant and a UV fluorescent lamp as a light source (365 nm). Both catalysts have shown very similar properties in the photocatalytic degradation of SMX. Special attention has been given to the effect of the irradiation time, pH, and pollutant concentration. No mass-transfer limitations are observed. The degradation of SMX is accelerated at low concentration, and the photocatalytic degradation kinetics obey the Langmuir–Hinshelwood model, allowing the adsorption and apparent rate constants to be determined for both catalysts.     

环境中抗生素及其生态毒性效应研究进展

近年来,越来越多的抗生素类药物用于在医疗、畜禽和水产养殖业。由于其机体代谢率低,大部分以原药或代谢物的形式经由尿液和粪便排出体外进入环境中,造成抗生素在水体和土壤等环境介质中的残留。这些残留的抗生素会导致潜在的环境风险,其中最严重的是会诱发和传播各类抗生素抗性基因(antibiotic resistance genes,ARGs),进而对人类健康产生威胁。本文介绍了环境中抗生素的来源,归趋和残留状况,并且对其所引起的生态毒性效应以及ARGs进行总结,最后指出了目前研究中存在的问题,并对未来研究进行了展望。     

我国养猪业废弃物中四环素类、磺胺类抗生素及相关抗性基因污染研究进展

我国是世界养猪第一大国,生猪饲养量和猪肉产量均位居世界第一。养猪业每年所产生的粪便、废水中含有大量畜用抗生素及其代谢产物,使养猪业废弃物成为环境中重要的抗生素污染源之一,随之产生的抗性基因污染及传播问题也不容忽视。本文结合近年来国内外的研究数据,对我国养猪业废弃物中四环素类、磺胺类抗生素及其相关抗性基因的检测方法、污染状况及影响抗性基因传播的因素进行了分析,并基于控制我国养猪行业抗生素及抗性基因污染的目的,提出了今后的研究重点。