保健食品中牛磺酸检测方法的研究

发布时间：2019-06-03 21:59

【摘要】：研究背景:随着市场经济的快速健康发展,食品类型日益增多,保健食品相继涌入市场。保健食品是食品的一大分支,针对特定的人群,具有调节人体多种功能的特性。但是目前国家对食品安全方面监督管理制度尚且不够健全,市场上出现了虚假伪食品,其中各类食品添加剂所占的比重比较大。比如瘦肉精,周黑鸭,汽水包,毒火腿等。影响人体健康的添加剂引起大众的恐慌。牛磺酸作为一种食品添加剂,出现在各类保健食品中的次数逐渐增多。但是,保健食品所含牛磺酸的量与标签是否相符,已经成为大众关心的问题,目前国标法处理过程较为复杂,因此,需要建立检测方法对特殊保健食品进行相关系统检测与分析研究。目的:由于国标和国内外文献对牛磺酸的前处理方法比较繁琐,根据牛磺酸的特性,尝试用不同溶剂对比进行提取,对样品进行不同比例倍数稀释,简化前处理过程,建立两种不同检测方法:超高效液相色谱-蒸发光散射检测(UPLC-ESLD)和液相色谱-串联质谱(LC-MS/MS)分析,对不同剂型保健食品中牛磺酸的含量进行安全性分析及检测,为今后相关的研究工作提供技术支持。方法:主要从提取方法、提取溶剂、色谱柱、流动相的浓度等几个方面进行一定的优化。建立用“超高效液相色谱-蒸发光散射器”检测13种不同批次保健食品中牛磺酸含量的方法;建立“液相色谱-串联质谱”检测12种不同批次保健食品中牛磺酸含量的方法,并通过精密度、稳定性实验来验证这两种方法。结果:1.利用超高效液相-蒸发光散射检测技术,简化了保健食品中牛磺酸的前处理方法,提取溶剂为乙腈-水(1:9体积比),根据样品含量进行稀释,待测物的提取率均在80%以上;采用Waters BEH Amide(50 mm×2.1 mm,1.7μm)色谱柱,流动相采用0.1%甲酸和乙腈水。样品在0.10~2.0 mg/m L范围内显示出稳定地线性关系。在不同添加水平下,保健食品的加标回收率范围在98.5%~100.7%之间,定量限为0.1mg/m L,相对标准偏差(RSD)在0.48%~1.29%范围内,结果表明,超高效液相色谱蒸发光散射检测技术可以提高检测效率和准确性。2.利用液相色谱串联质谱检测技术,采用ESI和MRM方式进行测定分析,简化了不同批次保健食品中牛磺酸前处理方法,选用乙腈-水(1:9体积比)作为提取剂,采用乙腈-水作为洗脱体系。检测样品在0.01~2.0μg/m L范围内显示了稳定的线性关系,在不同添加水平下,保健食品的回收率处在97.5%~100.8%范围内,定量限为1.0mg/kg,相对标准偏差(RSD)在0.67%~3.9%之间。该检测方法提高了检测12种保健食品中牛磺酸含量的速率和准确度。结论:1.建立了超高效液相色谱-蒸发光散射和液相色谱-串联质谱检测牛磺酸的方法。操作简便,高效灵敏,可以满足日常其它保健食品检测。为保健食品中牛磺酸的标准测定方法的制定和修订提供参考依据。2.与国标法相比,简化了保健食品中牛磺酸含量的前处理方法,避免了国标中的复杂的衍生法,节省成本,简单安全环保。3.两种检测方法存在较多的优势,灵敏度、精密度高,检测限低,检测效率高,为今后牛磺酸的检测工作提供技术支持。
[Abstract]:Research background: With the rapid and healthy development of the market economy, the food type is increasing, and the health food has successively poured into the market. The health food is a large branch of the food, and has the characteristics of regulating various functions of the human body for a specific group of people. However, in that present state, the supervision and management system for food safety is not sound enough, and the market has false pseudo-food, among which the proportion of all kinds of food additives is relatively large. Such as lean meat, Zhou black duck, steam-water bag, toxic ham, and the like. The additive that affects the health of the human body causes the general panic. As a kind of food additive, taurine has gradually increased in all kinds of health food. However, whether the amount of taurine contained in the health food is in accordance with the labeling, has become a concern of the general public, the process of the national standard method is more complex, therefore, it is necessary to establish a detection method for the detection and analysis of the relevant system of the special health food. Objective: Because of the complex of the national standard and the domestic and foreign documents on the pretreatment of taurine, according to the characteristics of taurine, the extraction is carried out with different solvents, the sample is diluted by multiple times, the pretreatment process is simplified, and two different detection methods are established: The content of taurine in different dosage forms of health food was analyzed and tested by ultra-high performance liquid chromatography-evaporative light scattering detection (UPLC-ESSLD) and liquid chromatography-tandem mass spectrometry (LC-MS/ MS). Methods: The extraction method, extraction solvent, chromatographic column and the concentration of mobile phase were optimized. A method for detecting the content of taurine in 13 different batches of health-care food was established by using ultra-high performance liquid chromatography-evaporative light-scattering device. The method for detecting the content of taurine in 12 different batches of health-care food was established by HPLC-tandem mass spectrometry, and the two methods were verified by precision and stability experiments. Results:1. The pre-treatment method of taurine in the health food is simplified by using the ultra-high performance liquid-phase-evaporation light scattering detection technology, the extraction solvent is acetonitrile-water (1:9 volume ratio), the sample content is diluted, the extraction rate of the object to be tested is more than 80 percent, and the Waters BEH Amde (50 mm-2.1mm) is adopted, 1.7. mu.m) Column with 0.1% formic acid and acetonitrile water in the mobile phase. The sample shows a stable linear relationship within the range of 0.10-2.0 mg/ m L. The recovery range of the health food is within the range of 98.5% ~ 100.7% and the relative standard deviation (RSD) is in the range of 0.48% ~ 1.29% at different addition levels. The results show that the ultra-high performance liquid chromatography evaporative light scattering detection technology can improve the detection efficiency and accuracy. The method of determination of taurine in different batches of health-care food was simplified by means of liquid chromatography-tandem mass spectrometry (LC-MS), and the pretreatment method of taurine in different batches of health-care food was simplified. Acetonitrile-water (1:9 volume ratio) was used as the extractant, and acetonitrile-water was used as the elution system. The stable linear relationship was shown in the range of 0.01-2.0. m u.g/ m L. The recovery rate of the health-care food was in the range of 97.5% ~ 100.8%, the limit of quantitation was 1.0 mg/ kg, and the relative standard deviation (RSD) was between 0.67% and 3.9%. The detection method improves the rate and the accuracy of detecting the content of taurine in 12 health foods. Conclusion:1. A method for detecting taurine by ultra-high performance liquid chromatography-evaporative light scattering and liquid chromatography-tandem mass spectrometry was established. Has the advantages of simple and convenient operation, high efficiency and sensitivity, and can meet the daily other health-care food detection. The reference is provided for the development and revision of the standard measuring method for taurine in the health food. Compared with the national standard method, the pretreatment method of the taurine content in the health food is simplified, the complex derivative method in the national standard is avoided, the cost is saved, the safety is simple and environment-friendly. The two detection methods have the advantages of more advantages, high sensitivity, high precision, low detection limit and high detection efficiency, and can provide technical support for detecting the taurine in the future.
【学位授予单位】：吉林大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS218;O657

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