幾種氟喹諾酮類藥物殘留和亞硝酸根的檢測新方法研究與應(yīng)用
發(fā)布時間:2018-06-06 16:44
本文選題:諾氟沙星 + 洛美沙星; 參考:《南華大學(xué)》2012年碩士論文
【摘要】:第一章分別介紹了氟喹諾酮類藥物諾氟沙星、洛美沙星和環(huán)境中污染物亞硝酸根的衛(wèi)生檢驗研究意義和當(dāng)前研究進(jìn)展,并分別簡要闡述了本課題所建立的諾氟沙星、洛美沙星和亞硝酸根三種物質(zhì)衛(wèi)生檢驗新方法的基本原理和定量測定的依據(jù)。 第二章為同時測定2種氟喹諾酮類抗生素的含量,研究了諾氟沙星(NFLX)和洛美沙星(LFLX)的同步熒光光譜及其一階導(dǎo)數(shù)同步熒光光譜,利用零交點法避免了它們之間的干擾。在pH=4.0的HAc-NaAc緩沖溶液中, λ=160nm的條件下,測定了諾氟沙星和洛美沙星的同步熒光光譜。進(jìn)一步對2種沙星的同步熒光光譜做一階導(dǎo)數(shù)處理,分別在NFLX和LFLX的導(dǎo)數(shù)同步熒光光譜為零的275.0nm和283.8nm處讀取另一種沙星的信號值。該值與濃度呈線性關(guān)系,,NFLX和LFLX的線性范圍分別為1.68×10~(-8)~5.64×10~(-6)mol·L~(-1),1.89×10~(-8)~6.19×10~(-6)mol·L~(-1);諾氟沙星和洛美沙星的檢出限分別是5.03×10~(-9)mol·L~(-1)和7.58×10~(-9)mol·L~(-1);RSD均在5%以下。方法簡單,靈敏度高,用于牛奶樣品中NFLX和LFLX的同時測定,結(jié)果滿意。本文對共發(fā)光的反應(yīng)機制和熒光增強的機理進(jìn)行了探討。 第三章根據(jù)諾氟沙星的分子結(jié)構(gòu)中喹諾酮能夠吸收短波長的光,發(fā)出較長 波長的熒光的特征,同時利用稀土元素釔(Ⅲ)與NFLX形成配合物,能使其熒光強度顯著增加。因此,建立釔(Ⅲ)離子增敏測定痕量諾氟沙星的分析方法。 在優(yōu)化的實驗條件下,用1cm石英比色池在激發(fā)和發(fā)射波長分別為275nm和429nm處測定其熒光強度;諾氟沙星在5.10×10~(-9)~5.64×10~(-6)mol·L~(-1)濃度范圍內(nèi)與體系的熒光強度呈良好的線性關(guān)系,相關(guān)系數(shù)為0.9993,檢出限為1.52×10~(-9)mol·L~(-1)(S/N=3);同時試驗了常見金屬離子及有機物質(zhì)對其測定的干擾,進(jìn)行了在牛奶樣品和藥物膠囊樣品的回收試驗,回收率在94.0%~105.0%之間,RSD在5%以內(nèi),結(jié)果令人滿意。該方法操作簡單、檢測限低的特點。 第四章在鹽酸介質(zhì)中,羅丹明G (Rhodamine G, RhG)的分子共振熒光信號強,發(fā)射峰尖而對稱,受干擾因素少;趤喯跛岣艽呋疜BrO_3氧化RhG的反應(yīng),建立了催化動力學(xué)共振熒光分析法測定痕量NO2-?疾炝梭w系熒光強度減弱值(ΔF)的影響因素,優(yōu)化了反應(yīng)條件。最大共振熒光峰位于540nm波長處,NO_2-在4.20~56.00μg·L~(-1)范圍內(nèi)與ΔF呈良好的線性關(guān)系,方法檢出限為1.65μg·L~(-1)。本方法用于環(huán)境水樣中NO_2-的測定,RSD小于5.0%,樣品加標(biāo)回收率為98.84%~104.33%。該方法靈敏,結(jié)果準(zhǔn)確,簡便易行,應(yīng)用于環(huán)境水樣的檢測,結(jié)果滿意。
[Abstract]:In the first chapter, the significance and progress of the hygienic test of norfloxacin, lomefloxacin and nitrite in the environment were introduced, and the norfloxacin, which was established in this paper, was briefly described. The basic principle and the basis for quantitative determination of three new methods for hygienic examination of Lomefloxacin and nitrite. Chapter 2 is the simultaneous determination of two fluoroquinolones antibiotics. The synchronous fluorescence spectra of norfloxacin (NFLX) and lomefloxacin (LFLX) and their first derivative synchronous fluorescence spectra were studied. The interference between them was avoided by zero intersection method. The synchronous fluorescence spectra of norfloxacin and lomefloxacin were determined in HAc-NaAc buffer solution with pH = 4.0 at 160 nm. Furthermore, the synchronous fluorescence spectra of two species of floxacin were treated with the first derivative, and the signal values of the other species were read at 275.0nm and 283.8nm, where the derivative synchronous fluorescence spectra of NFLX and LFLX were zero, respectively. The linear ranges of NFLX and LFLX were 1.68 脳 10 ~ (-8) ~ (-8) and 5.64 脳 10~(-6)mol ~ (-1), respectively. The detection limits of norfloxacin and lomefloxacin were 5.03 脳 10~(-9)mol L ~ (-1) and 7.58 脳 10~(-9)mol ~ (-1), respectively, and the detection limits of norfloxacin and lomefloxacin were less than 5%. The method is simple and sensitive, and has been applied to the simultaneous determination of NFLX and LFLX in milk samples with satisfactory results. The mechanism of co-luminescence and the mechanism of fluorescence enhancement are discussed in this paper. In chapter 3, according to the characteristics of long wavelength fluorescence, quinolones can absorb the light of short wavelength in the molecular structure of norfloxacin. At the same time, the complex of yttrium (鈪
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