本文選題：解吸附電暈束離子化 + 離子阱質(zhì)譜　； 參考：《湖南師范大學(xué)》2013年碩士論文

【摘要】：目前,對(duì)保健食品和中成藥中違禁藥物進(jìn)行檢測(cè)多依靠液相色譜、高效液相色譜-質(zhì)譜聯(lián)用法等,這些方法測(cè)定前需對(duì)樣品進(jìn)行前處理,耗時(shí)較長(zhǎng),在實(shí)際大批量商品篩選時(shí)不可操作。 敞開(kāi)式離子化技術(shù)成為質(zhì)譜技術(shù)的研究熱點(diǎn)和前沿領(lǐng)域,此技術(shù)可在無(wú)需樣品預(yù)處理的條件下對(duì)復(fù)雜基體樣品中的痕量待測(cè)物進(jìn)行直接離子化,極大的提高了質(zhì)譜分析的效率。本文以市場(chǎng)上常見(jiàn)的保健食品和中成藥對(duì)研究對(duì)象,利用實(shí)驗(yàn)室自行研制的解吸附電暈束離子化技術(shù)對(duì)其中可能添加的違禁藥物進(jìn)行快速檢測(cè),并研究了快速初篩過(guò)程中的基質(zhì)效應(yīng)。其主要內(nèi)容如下： 1.綜述保健食品和中成藥中違禁藥物的添加現(xiàn)狀以及對(duì)消費(fèi)者造成的危害。通過(guò)與常用的違禁藥物檢測(cè)方法比較,研究常壓直接離子化技術(shù)在違禁藥物檢測(cè)領(lǐng)域具有的優(yōu)勢(shì)。 2.在優(yōu)化的實(shí)驗(yàn)條件下,利用解吸附電暈束離子源(DCBI)結(jié)合離子阱質(zhì)譜快速檢測(cè)了3個(gè)磷酸二酯酶5(PDE5)抑制劑伐地那非、西地那非、他達(dá)拉非。采用一級(jí)質(zhì)譜篩選,二級(jí)質(zhì)譜確證,對(duì)樣品中非法添加物進(jìn)行定性鑒別；通過(guò)二級(jí)特征碎片離子進(jìn)行半定量分析,與傳統(tǒng)高效液相色譜-紫外(HPLC-UV)檢測(cè)法作對(duì)比,研究了3個(gè)PDE5抑制劑的二級(jí)質(zhì)譜裂解規(guī)律。實(shí)現(xiàn)了分析速度快、樣品用量少、無(wú)需使用其他化學(xué)試劑、無(wú)污染的檢測(cè)。 3.在優(yōu)化的實(shí)驗(yàn)條件下,建立了DCBI-MS法快速檢測(cè)9種β2-受體激動(dòng)劑。利用一級(jí)質(zhì)譜篩選,二級(jí)質(zhì)譜確證,對(duì)樣品中非法添加物進(jìn)行定性鑒別；并通過(guò)二級(jí)特征碎片離子進(jìn)行半定量分析。本方法無(wú)需復(fù)雜的前處理過(guò)程,簡(jiǎn)便、快速、靈敏度高,可用于止咳平喘類藥物中β2-受體激動(dòng)劑違禁添加的快速定性及半定量檢測(cè)。 4.以市場(chǎng)上常見(jiàn)違禁添加的抗疲勞保健食品為研究對(duì)象,選取不同劑型的空白樣品(片劑,丸劑,膠囊,合劑,酒劑,糖漿,口服液),通過(guò)空白加標(biāo)法測(cè)定基質(zhì)對(duì)3個(gè)PDE5抑制劑伐地那非、西地那非、他達(dá)拉非的檢測(cè)限及半定量分析的影響。此研究結(jié)果為DCBI-MS法測(cè)定不同劑型不同輔料中其他目標(biāo)物的前處理過(guò)程的必要性提供了參考依據(jù)。
[Abstract]:At present, the detection of illegal drugs in health food and Chinese patent medicine mostly depends on liquid chromatography, high performance liquid chromatography-mass spectrometry and so on. In the actual mass selection of goods can not be operated. The open ionization technology has become the hot spot and frontier of mass spectrometry technology. This technology can directly ionize trace samples in complex matrix samples without sample pretreatment, which greatly improves the efficiency of mass spectrometry analysis. In this paper, the common health food and Chinese patent medicine in the market were used to detect the possible illegal drugs by using the desorption corona beam ionization technology developed by the laboratory. The matrix effect in the process of rapid screening was studied. Its main contents are as follows: 1. This paper reviews the status quo of illicit drugs in health food and Chinese patent medicine and the harm to consumers. The advantages of atmospheric direct ionization in the field of illicit drug detection were studied by comparing with the commonly used methods of drug detection. 2. Under the optimized experimental conditions, three phosphodiesterase 5 (PDE5) inhibitors, Vardenafil, sildenafil, and tadalafil, were rapidly detected by desorption corona beam ion source (DCBI) and ion trap mass spectrometry. The illegal additives in the samples were qualitatively identified by first stage mass spectrometry screening and confirmed by secondary mass spectrometry, and compared with the traditional high performance liquid chromatography-UV (HPLC-UV) detection method by semi-quantitative analysis of secondary characteristic fragment ions. The cleavage of three PDE5 inhibitors by secondary mass spectrometry was studied. Rapid analysis, less sample consumption, no use of other chemical reagents, no pollution detection. 3. Under the optimized experimental conditions, a DCBI-MS method was established for the rapid detection of 9 尾 2 receptor agonists. The illegal additives in the samples were qualitatively identified by first-order mass spectrometry screening and confirmed by second-order mass spectrometry, and semi-quantitative analysis was carried out by secondary characteristic fragment ions. The method is simple, rapid and sensitive without complicated pretreatment process. It can be used for rapid qualitative and semi-quantitative detection of 尾 _ 2-receptor agonists in cough and antiasthmatic drugs. 4. Taking anti-fatigue health food as the research object, the blank samples of different dosage forms (tablets, pills, capsules, mixture, liquor, syrup) were selected. The effect of substrate on the detection limits and semi-quantitative analysis of three PDE5 inhibitors, vardenafil, sildenafil, and tadalafil, was determined by blank plus standard method. The results of this study provide a reference for the determination of other objects in different dosage forms and excipients by DCBI-MS.
【學(xué)位授予單位】：湖南師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2013
【分類號(hào)】：R155.5;R286;O657.63

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