【摘要】：藥品和個人護(hù)理用品(Pharmaceutical and Personal Care Products,PPCPs),作為人類生活的必需品,隨著科技發(fā)展和人類消費水平的提高,其應(yīng)用范圍和使用量也都日益增長。但也因此,隨著廢棄物的排放,PPCPs在環(huán)境中也一直存在,并以濃度低、數(shù)量多為特點。PPCPs的毒性主要以長期積累的慢性毒性為主,積累到一定程度才會顯示出來,是影響人類健康和環(huán)境安全的潛在威脅,因此,對PPCPs進(jìn)行有效的檢測很有必要。本研究針對環(huán)境與食品中的部分PPCPs的檢測方法進(jìn)行研究,在植物種植環(huán)境方面,對灌溉用再生水中的高含量污染物進(jìn)篩查與確證,并對易在種植土壤中積累的多環(huán)芳烴進(jìn)行檢測,在動物源食品安全方面,優(yōu)化了對于牛奶中頭孢菌素的檢測方法。主要工作內(nèi)容如下:1、本文對北京市兩條農(nóng)灌河流中再生水中存在的主要PPCPs類污染物進(jìn)行篩查和確證,利用固相萃取(SPE)的方法對再生水樣品進(jìn)行富集,超高效液相色譜-飛行時間質(zhì)譜(UPLC-Q-TOF)對樣品中的污染物進(jìn)行篩查,通過數(shù)據(jù)庫和文獻(xiàn)比對等方法,并利用UPLC-MS/MS進(jìn)行驗證,最終確定出阿奇霉素、甘寶素、氧氟沙星、美托洛爾、普羅帕酮、羅紅霉素、替米沙坦、左西替利嗪、厄貝沙坦、莠去津、自克威、撲草凈、烯酰嗎啉、羅丹明B、格列齊特和三丁氧基乙基磷酸酯(TBEP)共16種含量較高的PPCPs。利用UPLC-MS/MS對其進(jìn)行定量評估,方法檢出限為0.2ng/L～8ng/L,定量限為0.3ng/L～10ng/L,線性相關(guān)系數(shù)(R2)大于0.99,精密度(RSD)小于15%。再生水樣品中存在的PPCPs類污染物最大含量范圍為6ng/L～20.5μg/L。2、對于河流周邊土壤的考察,重點放在持久性有機污染物多環(huán)芳烴(PAHs)的檢測。本文利用微波輔助萃取(MAE)方法對土壤中的萘、蒽、菲、芘、苊、(?)、芴、苊烯、熒蒽、二苯蒽、苯并(a)蒽、苯并(a)芘、苯并(g,h,i)芘,苯并(k)熒蒽,苯并(b)熒蒽和茚并(1,2,3-CD)芘共16種PAHs進(jìn)行提取,并通過響應(yīng)曲面法(RSM)對提取條件進(jìn)行優(yōu)化,最佳提取條件為萃取溫度100℃、萃取時間16min和萃取劑用量15mL。通過超臨界流體色譜(UPCC)對其進(jìn)行定量檢測,方法檢出限為2.5μg/Kg～7.5μg/Kg,定量限為5μg/Kg～15μg/Kg,線性相關(guān)系數(shù)(R2)大于0.99,RSD小于18.9%。土壤樣品中存在的PAHs類物質(zhì)僅檢測到苯并(a)芘在土壤粒子中有較強的吸附能力,其在土壤中的含量達(dá)到596μg/Kg。3、牛奶作為動物源性食品,本文還利用SPE方法對牛奶中的頭孢菌素(AmpC)類抗生素進(jìn)行提取凈化,建立并優(yōu)化了使用弱陰離子交換(WAX)固相萃取柱同時富集檢測頭孢米諾鈉、頭孢氨噻肟、頭孢哌酮、頭孢克肟、頭孢他美酯、頭孢噻酚鈉和頭孢呋辛7種物質(zhì)的檢測方法。利用UPLC-MS/MS進(jìn)行定量分析,方法檢出限為0.05μg/L～2.4μg/L,定量限為0.1μg/L～3.2μg/L,加標(biāo)回收率在47.63%～114.62%,線性相關(guān)系數(shù)(R2)大于 0.99,RSD 小于 13.66%。對市售的牛奶樣品進(jìn)行檢測,并沒有發(fā)現(xiàn)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，

本文編號：2363090