本文關(guān)鍵詞： 敞開式質(zhì)譜 紙噴霧技術(shù) 保健食品 違禁添加 快速檢測 疏水紙　出處：《湖南師范大學(xué)》2016年碩士論文　論文類型：學(xué)位論文

【摘要】：當(dāng)代社會,保健食品的迅猛發(fā)展使得市面上出現(xiàn)了大量虛假宣傳的各種濫竽充數(shù)的假冒偽劣產(chǎn)品,使得相關(guān)部門對保健品行業(yè)的監(jiān)督管理出現(xiàn)漏洞。與此同時,政府部門乃至整個社會已經(jīng)開始熱切關(guān)注整個保健食品行業(yè)的安全問題�，F(xiàn)代社會面臨的難題主要是:如何正確引導(dǎo)消費者認(rèn)識保健食品;如何有效防止違禁添加藥物;相關(guān)部門如何管制和掌控整個保健食品的市場等。以往用來檢測保健食品中的違禁添加藥物的傳統(tǒng)方法如高效液相色譜法和色譜-質(zhì)譜聯(lián)用法靈敏度高,測定準(zhǔn)確,但是耗時較長,前處理過程復(fù)雜,并且流動相需要大量有機(jī)試劑,無論從經(jīng)濟(jì)還是環(huán)保的角度,這兩種方法都不適用于市面上大批量樣品的快速篩查和實際鑒定�？萍嫉陌l(fā)展也帶動了質(zhì)譜技術(shù)的發(fā)展,作為一種新型的離子化技術(shù),敞開式離子化質(zhì)譜技術(shù)不僅分析速度快,避免了繁雜而耗時的前處理過程,而且測定結(jié)果準(zhǔn)確可靠,對于保健食品中的復(fù)雜成分,仍然可以將其準(zhǔn)確定性分析檢測,目前敞開式的離子化質(zhì)譜已經(jīng)逐漸代替?zhèn)鹘y(tǒng)的質(zhì)譜法而成為質(zhì)譜分析中不可缺少的一種新的離子化方法。紙噴霧離子化是敞開式質(zhì)譜技術(shù)中的一個新的分支,其簡單、易操作、溶劑消耗少、價格低廉,具有很好的發(fā)展前景和廣闊的應(yīng)用領(lǐng)域。近幾年,國內(nèi)外紙噴霧離子化技術(shù)已被廣泛應(yīng)用于環(huán)境、食品、藥品及公共安全等多個領(lǐng)域的研究。本文的主要內(nèi)容如下:(1)利用紙噴霧離子化技術(shù)對男性抗疲勞保健食品中的違禁添加物的定性定量分析檢測。在正離子模式下,在3.5 KV電壓下,以100℃為離子源溫度,以甲醇為溶劑,每次重復(fù)進(jìn)樣20μL,先對標(biāo)準(zhǔn)品進(jìn)行定位,得到目標(biāo)物的質(zhì)譜圖,然后對待測樣品進(jìn)行定性分析,最后,以待測物質(zhì)與內(nèi)標(biāo)物西布曲明的信號強(qiáng)度比為參數(shù)進(jìn)行定量分析,結(jié)果表明該方法對市售保健食品中的3種磷酸二酯酶5的半定量分析結(jié)果可信可靠3種PDE5抑制劑在5.00~56.00 mg·L-1范圍內(nèi)線性相關(guān),R2均大于0.99,檢測限低至0.1 mg·L-1。此方法前處理過程簡單快速,溶劑消耗少,適用于市場上保健食品的大批量快速篩查,雖然檢測結(jié)果與高效液相色譜相比并非完全一致,但是紙噴霧離子化質(zhì)譜法可以作為一種半定量分析方法,作為一種初步篩查手法應(yīng)用到保健食品的違禁添加檢測中。(2)在優(yōu)化的實驗條件下,對減肥類保健食品中違禁添加物進(jìn)行快速檢測。應(yīng)用紙噴霧離子化技術(shù),包括西布曲明、單去甲基西布曲明、雙去甲基西布曲明、酚酞及芬氟拉明5種常見的非法添加成分被成功檢出。在正離子模式下,先對標(biāo)準(zhǔn)品進(jìn)行定位,然后對待測樣品進(jìn)行定性分析,最后,以待測物質(zhì)與內(nèi)標(biāo)物西地那非的信號強(qiáng)度比為參數(shù)進(jìn)行定量分析,結(jié)果表明該方法對5種違禁物質(zhì)在市售減肥類保健食品中的半定量分析結(jié)果可信。(3)建立了在負(fù)電壓模式下,以疏水紙為載體的紙噴霧質(zhì)譜分析方法,對比了分別在負(fù)電壓模式和正電壓模式下,三類包括有機(jī)酸、有機(jī)胺和氨基酸在內(nèi)的物質(zhì),然后分別以疏水紙和普通紙為載體,進(jìn)行離子化質(zhì)譜分析。經(jīng)過比較,最后將疏水紙應(yīng)用于市售降血糖類保健食品中磺脲類藥物的快速檢測及半定量分析。分別檢測了市面上暢銷的各種不同劑型的降糖類保健食品中的6種磺脲類物質(zhì)。
[Abstract]:In modern society, the rapid development of health food has appeared in a variety of more than a large number of false propaganda of shoddy products on the market, the relevant departments of supervision and management of the health care industry loopholes. At the same time, government departments and the whole society has begun to focus on safety in the whole heat cutting health food industry. Modern society is facing the main problem how to correctly guide the consumer awareness of health food; how to effectively prevent the prohibited drugs; the relevant departments on how to control and control of the health food market. It used to traditional methods of detection in health food prohibited drugs such as HPLC and LC-MS determination of high sensitivity, accurate but time-consuming first, the complex process, and the mobile phase requires a lot of organic reagents, either from the economic and environmental protection angle, the two Rapid screening and identification of the actual methods are not applicable to the market of large quantities of samples. The development of science and technology has also led to the development of mass spectrometry technology, as a new ionization technique, open ionization mass spectrometry technology not only fast analysis, to avoid the pretreatment process is complicated and time-consuming, and the results were accurate and reliable, for the complex composition of health food, it can still be accurate qualitative analysis and detection, the current open mass spectrometry ionization mass spectrometry has been gradually replacing the traditional style and become indispensable in mass spectrometric analysis a new ionization method. The paper spray ionization is open a new branch in the simple type of mass spectrometry. Easy operation, less solvent consumption, low price, with good prospects and wide application fields. In recent years, domestic and foreign paper spray ionization technique has been widely used in environmental, food Study on multiple areas of goods, drugs and public security and so on. The main contents of this paper are as follows: (1) analyzed by electrospray ionization detection. Paper qualitative and quantitative on male health food illegal additives anti fatigue in the positive ion mode, under the voltage of 3.5 KV, to 100 degrees for the ion source temperature, to methanol as solvent, each repeated injection of 20 L, the first location of the standard mass spectra obtained of the object, and then to be measured by qualitative analysis, finally, with the test signal intensity of standard substance and sibutramine ratio parameters were quantitatively analyzed and the results show that the semi quantitative analysis of the method for the market 3 kinds of phosphodiesterase in health food 5 reliable 3 kinds of PDE5 inhibitors in 5.00~56.00 mg, within the linear range of L-1, R2 were higher than 0.99, the detection limit is as low as 0.1 mg L-1. this method pretreatment process is simple and fast, less solvent consumption On the market, suitable for rapid screening of large quantities of health food, although the test results with high performance liquid chromatography compared is not exactly the same, but the paper spray ionization mass spectrometry can be used as a semi quantitative analysis method, detection added as a preliminary screening technique applied to health food illegal. (2) under the optimized experimental conditions under the fast detection of contraband in slimming foods additives. Application of paper spray ionization technique, including sibutramine, single demethylated sibutramine, dinor sibutramine, phenolphthalein and fenfluramine illegally added 5 kinds of components were successfully detected. In positive ion mode, first locate the standard, and then tested samples for qualitative analysis, finally, with the test signal intensity of standard substance and sildenafil ratio parameters for quantitative analysis, the results show that the method of 5 kinds of contraband In commercially available slimming health food in the semi quantitative analysis results. (3) established in negative voltage mode, the hydrophobic paper analysis method for paper carrier electrospray mass spectrometry, were compared respectively in the negative voltage mode and positive voltage mode, including three kinds of organic acids, amino acids, and organic amine the material, then the hydrophobic paper and plain paper as the carrier of ionization mass spectrometry analysis. By comparison, the hydrophobic paper applied to the commercially available analysis and semi quantitative rapid detection of sulfonylurea glucose in health food were detected. Hypoglycemic health food of different types on the market are sold in 6 kinds of sulfonylurea compounds.

【學(xué)位授予單位】：湖南師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O657.63;TS218
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本文編號：1528290