液相色谱与质谱联用对环境与食品中PPCPs类物质的筛查与检测
发布时间：2018-11-28 14:15
【摘要】：药品和个人护理用品(Pharmaceutical and Personal Care Products,PPCPs),作为人类生活的必需品,随着科技发展和人类消费水平的提高,其应用范围和使用量也都日益增长。但也因此,随着废弃物的排放,PPCPs在环境中也一直存在,并以浓度低、数量多为特点。PPCPs的毒性主要以长期积累的慢性毒性为主,积累到一定程度才会显示出来,是影响人类健康和环境安全的潜在威胁,因此,对PPCPs进行有效的检测很有必要。本研究针对环境与食品中的部分PPCPs的检测方法进行研究,在植物种植环境方面,对灌溉用再生水中的高含量污染物进筛查与确证,并对易在种植土壤中积累的多环芳烃进行检测,在动物源食品安全方面,优化了对于牛奶中头孢菌素的检测方法。主要工作内容如下:1、本文对北京市两条农灌河流中再生水中存在的主要PPCPs类污染物进行筛查和确证,利用固相萃取(SPE)的方法对再生水样品进行富集,超高效液相色谱-飞行时间质谱(UPLC-Q-TOF)对样品中的污染物进行筛查,通过数据库和文献比对等方法,并利用UPLC-MS/MS进行验证,最终确定出阿奇霉素、甘宝素、氧氟沙星、美托洛尔、普罗帕酮、罗红霉素、替米沙坦、左西替利嗪、厄贝沙坦、莠去津、自克威、扑草净、烯酰吗啉、罗丹明B、格列齐特和三丁氧基乙基磷酸酯(TBEP)共16种含量较高的PPCPs。利用UPLC-MS/MS对其进行定量评估,方法检出限为0.2ng/L～8ng/L,定量限为0.3ng/L～10ng/L,线性相关系数(R2)大于0.99,精密度(RSD)小于15%。再生水样品中存在的PPCPs类污染物最大含量范围为6ng/L～20.5μg/L。2、对于河流周边土壤的考察,重点放在持久性有机污染物多环芳烃(PAHs)的检测。本文利用微波辅助萃取(MAE)方法对土壤中的萘、蒽、菲、芘、苊、(?)、芴、苊烯、荧蒽、二苯蒽、苯并(a)蒽、苯并(a)芘、苯并(g,h,i)芘,苯并(k)荧蒽,苯并(b)荧蒽和茚并(1,2,3-CD)芘共16种PAHs进行提取,并通过响应曲面法(RSM)对提取条件进行优化,最佳提取条件为萃取温度100℃、萃取时间16min和萃取剂用量15mL。通过超临界流体色谱(UPCC)对其进行定量检测,方法检出限为2.5μg/Kg～7.5μg/Kg,定量限为5μg/Kg～15μg/Kg,线性相关系数(R2)大于0.99,RSD小于18.9%。土壤样品中存在的PAHs类物质仅检测到苯并(a)芘在土壤粒子中有较强的吸附能力,其在土壤中的含量达到596μg/Kg。3、牛奶作为动物源性食品,本文还利用SPE方法对牛奶中的头孢菌素(AmpC)类抗生素进行提取净化,建立并优化了使用弱阴离子交换(WAX)固相萃取柱同时富集检测头孢米诺钠、头孢氨噻肟、头孢哌酮、头孢克肟、头孢他美酯、头孢噻酚钠和头孢呋辛7种物质的检测方法。利用UPLC-MS/MS进行定量分析,方法检出限为0.05μg/L～2.4μg/L,定量限为0.1μg/L～3.2μg/L,加标回收率在47.63%～114.62%,线性相关系数(R2)大于 0.99,RSD 小于 13.66%。对市售的牛奶样品进行检测,并没有发现其中存在上述AmpC。
[Abstract]:Drugs and personal care products (Pharmaceutical and Personal Care Products,PPCPs), as a necessity of human life, with the development of science and technology and the improvement of human consumption, its application scope and usage are also increasing. However, with the discharge of wastes, PPCPs has always existed in the environment, and it is characterized by low concentration and large quantity. The toxicity of PPCPs is mainly chronic toxicity accumulated over a long period of time, and only when it accumulates to a certain extent can it be shown. It is a potential threat to human health and environmental safety, so it is necessary to detect PPCPs effectively. In this study, the detection method of partial PPCPs in environment and food was studied. In plant planting environment, the high content of pollutants in regenerated water for irrigation was screened and confirmed. The polycyclic aromatic hydrocarbons (PAHs) easily accumulated in the cultivated soil were detected and the method for the detection of cephalosporins in milk was optimized in the aspect of animal food safety. The main contents are as follows: 1. The main PPCPs pollutants in the regenerated water of two agricultural irrigation rivers in Beijing were screened and confirmed, and the samples were enriched by solid phase extraction (SPE). Ultrahigh performance liquid chromatography-time-of-flight mass spectrometry (UPLC-Q-TOF) was used to screen contaminants in the samples. By means of database and literature comparison, azithromycin and glycomycin were determined by UPLC-MS/MS. Ofloxacin, metoprolol, propafenone, roxithromycin, telmisartan, levocetirizine, irbesartan, atrazine, autoclave, propofol, enyl morpholine, Rhodamine B, Gliclazide and Tributoxyethyl Phosphate (TBEP) 16 kinds of PPCPs. with higher content The detection limit is 0.2 ng / L ~ (8) ng / L, the quantitative limit is 0.3 ng / L ~ (10) ng / L, the linear correlation coefficient (R ~ 2) is greater than 0.99, and the precision (RSD) is less than 15%. The maximum concentration range of PPCPs pollutants in reclaimed water samples was 6ng/L~20.5 渭 g / L ~ (2). The detection of polycyclic aromatic hydrocarbons (PAHs) in soils around rivers was emphasized. The microwave-assisted extraction of naphthalene, anthracene, phenanthrene, pyrene, acenaphthene, fluorene, acenaphthene, fluoranthene, diphenyl anthracene, benzo (a) pyrene, benzo (a) pyrene in soil was studied by microwave assisted extraction. Sixteen kinds of benzo (k) fluoranthene, benzo (b) fluoranthene and indeno 23-CD pyrene were extracted, and the extraction conditions were optimized by response surface method (RSM). The optimum extraction conditions were as follows: extraction temperature 100 鈩，
本文编号：2363090
[Abstract]:Drugs and personal care products (Pharmaceutical and Personal Care Products,PPCPs), as a necessity of human life, with the development of science and technology and the improvement of human consumption, its application scope and usage are also increasing. However, with the discharge of wastes, PPCPs has always existed in the environment, and it is characterized by low concentration and large quantity. The toxicity of PPCPs is mainly chronic toxicity accumulated over a long period of time, and only when it accumulates to a certain extent can it be shown. It is a potential threat to human health and environmental safety, so it is necessary to detect PPCPs effectively. In this study, the detection method of partial PPCPs in environment and food was studied. In plant planting environment, the high content of pollutants in regenerated water for irrigation was screened and confirmed. The polycyclic aromatic hydrocarbons (PAHs) easily accumulated in the cultivated soil were detected and the method for the detection of cephalosporins in milk was optimized in the aspect of animal food safety. The main contents are as follows: 1. The main PPCPs pollutants in the regenerated water of two agricultural irrigation rivers in Beijing were screened and confirmed, and the samples were enriched by solid phase extraction (SPE). Ultrahigh performance liquid chromatography-time-of-flight mass spectrometry (UPLC-Q-TOF) was used to screen contaminants in the samples. By means of database and literature comparison, azithromycin and glycomycin were determined by UPLC-MS/MS. Ofloxacin, metoprolol, propafenone, roxithromycin, telmisartan, levocetirizine, irbesartan, atrazine, autoclave, propofol, enyl morpholine, Rhodamine B, Gliclazide and Tributoxyethyl Phosphate (TBEP) 16 kinds of PPCPs. with higher content The detection limit is 0.2 ng / L ~ (8) ng / L, the quantitative limit is 0.3 ng / L ~ (10) ng / L, the linear correlation coefficient (R ~ 2) is greater than 0.99, and the precision (RSD) is less than 15%. The maximum concentration range of PPCPs pollutants in reclaimed water samples was 6ng/L~20.5 渭 g / L ~ (2). The detection of polycyclic aromatic hydrocarbons (PAHs) in soils around rivers was emphasized. The microwave-assisted extraction of naphthalene, anthracene, phenanthrene, pyrene, acenaphthene, fluorene, acenaphthene, fluoranthene, diphenyl anthracene, benzo (a) pyrene, benzo (a) pyrene in soil was studied by microwave assisted extraction. Sixteen kinds of benzo (k) fluoranthene, benzo (b) fluoranthene and indeno 23-CD pyrene were extracted, and the extraction conditions were optimized by response surface method (RSM). The optimum extraction conditions were as follows: extraction temperature 100 鈩，
本文编号：2363090
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