九种毒品及蜂蜜中5-羟甲基糠醛标准物质定值

发布时间：2018-11-03 20:05

【摘要】：随着我国经济和社会的快速发展,人类的身心健康问题受到越来越多的关注,涉及此问题的相关物质分析检测急剧增加,对其检测技术水平的标准与要求也越来越高。标准物质能够保证测定结果的准确度、实验方法的可靠性,其使用量也随之增加。论文针对国内毒品标准物质的空白及法庭领域毒品犯罪案件证据的缺乏性,本文结合国内相关的研究技术基础,从毒品成分量测量能力着手,开展了甲基苯丙胺、氯胺酮、吗啡、可卡因、杜冷丁、海洛因、美沙酮、地西泮、艾司唑仑九种纯度标准物质的定值工作。毒品样品的主成分通过红外光谱、质谱和熔点法对其进行定性分析,纯度定值分析方法则采用色谱法(液相和气相)及差示扫描量热法等手段,同时完成水分、无机离子和灰分含量的测定,随机抽样检验毒品样品的均匀性、稳定性,计算总的不确定度。结果表明九种毒品样品的主成分与相应标准物质相符,定值方法测得的纯品样品纯度都在99%以上,瓶间和瓶内的均匀性良好,稳定期在1年以上。毒品标准物质定值建立了毒品成分量的测量方法以及相应的国家标准物质,一方面为法庭科学领域的量刑等服务,另一方面提高了我国法庭科学领域毒品成分测量在国际上的地位,使其测量结果能够得到国际的认可,为我国在国际上相关领域的纠纷提供了技术支撑。蜂蜜作为具有较高营养价值的天然产品广泛被社会大众所认可,但是蜂蜜中5-羟甲基糠醛的产生对人体有一定的危害作用。为了控制蜂蜜的质量和保障人类身体健康,本文对蜂蜜中5-HMF基体标准物质的定值过程进行了研究。由于蜂蜜基体的复杂性,对样品前处理方法进行了分析研究,选择Strata-X反相聚合物吸附剂萃取柱对样品进行固相萃取,方法回收率在98.8%-100.5%范围内。采用高效液相色谱法(外标法)和同位素稀释质谱法(内标法)两种方法同时对蜂蜜中低、中、高浓度的5-HMF含量进行定值分析,浓度分别为10.8μg/g、26.9μg/g和66.4μg/g,按照国家标准物质规范要求检验蜂蜜样品的均匀性良好,稳定期至少半年,同时进行不确定度评定。蜂蜜中5-羟甲基糠醛基体标准物质的定值,为蜂产品行业的食品质量安全提供了可靠的技术支持。
[Abstract]:With the rapid development of economy and society in China, more and more attention has been paid to the physical and mental health of human beings. The standard material can guarantee the accuracy of the determination results and the reliability of the experimental method. Aiming at the blank of domestic drug standard material and the lack of evidence in the field of drug crime in the court field, this paper combines the domestic relevant research technical foundation, from the drug component measurement ability, carried out the methamphetamine, ketamine, Determination of nine purity reference substances for morphine, cocaine, Durantin, heroin, methadone, diazepam and eszolam. The principal components of drug samples were qualitatively analyzed by IR, mass spectrometry and melting point method. The purity determination methods were chromatography (liquid phase and gas phase) and differential scanning calorimetry (DSC). Determination of inorganic ions and ash content, random sampling to test the homogeneity and stability of drug samples, calculation of total uncertainty. The results showed that the principal components of the nine kinds of drug samples were consistent with the corresponding reference materials. The purity of the pure samples determined by the method was above 99%. The homogeneity between bottles and bottles was good, and the stability period was more than one year. The determination of the value of the drug standard material establishes the measurement method of the drug component and the corresponding national standard material. On the one hand, it serves the sentencing in the field of court science and so on. On the other hand, it improves the international status of drug composition measurement in the field of forensic science in China, and makes the result of the measurement can be recognized internationally, which provides a technical support for the disputes in the related fields of our country. Honey as a natural product with high nutritional value is widely recognized by the public, but the production of 5-hydroxymethylfurfural in honey has a certain harm to human body. In order to control the quality of honey and ensure human health, the determination process of 5-HMF matrix reference material in honey was studied in this paper. Because of the complexity of honey matrix, the sample pretreatment method was analyzed and studied. Strata-X reverse polymer adsorbent extraction column was selected for solid phase extraction of the sample. The recovery of the method was in the range of 98.8- 100.5%. High performance liquid chromatography (external standard method) and isotope dilution mass spectrometry (internal standard method) were used to determine the content of 5-HMF in honey. The concentration of 5-HMF was 10.8 渭 g / g, respectively. 26.9 渭 g / g and 66.4 渭 g / g, the homogeneity of honey samples is good according to the national standard material specification, the stability period is at least half a year, and the uncertainty is evaluated at the same time. The determination of 5-hydroxymethylfurfural matrix reference material in honey provides reliable technical support for food quality and safety in bee products industry.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R155.5;S896.1

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