保健食品中违禁添加物的敞开式质谱分析

发布时间：2018-02-24 01:06

  本文关键词： 敞开式质谱 纸喷雾技术 保健食品 违禁添加 快速检测 疏水纸　出处：《湖南师范大学》2016年硕士论文　论文类型：学位论文

【摘要】：当代社会,保健食品的迅猛发展使得市面上出现了大量虚假宣传的各种滥竽充数的假冒伪劣产品,使得相关部门对保健品行业的监督管理出现漏洞。与此同时,政府部门乃至整个社会已经开始热切关注整个保健食品行业的安全问题。现代社会面临的难题主要是:如何正确引导消费者认识保健食品;如何有效防止违禁添加药物;相关部门如何管制和掌控整个保健食品的市场等。以往用来检测保健食品中的违禁添加药物的传统方法如高效液相色谱法和色谱-质谱联用法灵敏度高,测定准确,但是耗时较长,前处理过程复杂,并且流动相需要大量有机试剂,无论从经济还是环保的角度,这两种方法都不适用于市面上大批量样品的快速筛查和实际鉴定。科技的发展也带动了质谱技术的发展,作为一种新型的离子化技术,敞开式离子化质谱技术不仅分析速度快,避免了繁杂而耗时的前处理过程,而且测定结果准确可靠,对于保健食品中的复杂成分,仍然可以将其准确定性分析检测,目前敞开式的离子化质谱已经逐渐代替传统的质谱法而成为质谱分析中不可缺少的一种新的离子化方法。纸喷雾离子化是敞开式质谱技术中的一个新的分支,其简单、易操作、溶剂消耗少、价格低廉,具有很好的发展前景和广阔的应用领域。近几年,国内外纸喷雾离子化技术已被广泛应用于环境、食品、药品及公共安全等多个领域的研究。本文的主要内容如下:(1)利用纸喷雾离子化技术对男性抗疲劳保健食品中的违禁添加物的定性定量分析检测。在正离子模式下,在3.5 KV电压下,以100℃为离子源温度,以甲醇为溶剂,每次重复进样20μL,先对标准品进行定位,得到目标物的质谱图,然后对待测样品进行定性分析,最后,以待测物质与内标物西布曲明的信号强度比为参数进行定量分析,结果表明该方法对市售保健食品中的3种磷酸二酯酶5的半定量分析结果可信可靠3种PDE5抑制剂在5.00~56.00 mg·L-1范围内线性相关,R2均大于0.99,检测限低至0.1 mg·L-1。此方法前处理过程简单快速,溶剂消耗少,适用于市场上保健食品的大批量快速筛查,虽然检测结果与高效液相色谱相比并非完全一致,但是纸喷雾离子化质谱法可以作为一种半定量分析方法,作为一种初步筛查手法应用到保健食品的违禁添加检测中。(2)在优化的实验条件下,对减肥类保健食品中违禁添加物进行快速检测。应用纸喷雾离子化技术,包括西布曲明、单去甲基西布曲明、双去甲基西布曲明、酚酞及芬氟拉明5种常见的非法添加成分被成功检出。在正离子模式下,先对标准品进行定位,然后对待测样品进行定性分析,最后,以待测物质与内标物西地那非的信号强度比为参数进行定量分析,结果表明该方法对5种违禁物质在市售减肥类保健食品中的半定量分析结果可信。(3)建立了在负电压模式下,以疏水纸为载体的纸喷雾质谱分析方法,对比了分别在负电压模式和正电压模式下,三类包括有机酸、有机胺和氨基酸在内的物质,然后分别以疏水纸和普通纸为载体,进行离子化质谱分析。经过比较,最后将疏水纸应用于市售降血糖类保健食品中磺脲类药物的快速检测及半定量分析。分别检测了市面上畅销的各种不同剂型的降糖类保健食品中的6种磺脲类物质。
[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.

【学位授予单位】：湖南师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.63;TS218
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本文编号：1528290