【摘要】：隨著我國經(jīng)濟和社會的快速發(fā)展,人類的身心健康問題受到越來越多的關(guān)注,涉及此問題的相關(guān)物質(zhì)分析檢測急劇增加,對其檢測技術(shù)水平的標準與要求也越來越高。標準物質(zhì)能夠保證測定結(jié)果的準確度、實驗方法的可靠性,其使用量也隨之增加。 論文針對國內(nèi)毒品標準物質(zhì)的空白及法庭領(lǐng)域毒品犯罪案件證據(jù)的缺乏性,本文結(jié)合國內(nèi)相關(guān)的研究技術(shù)基礎(chǔ),從毒品成分量測量能力著手,開展了甲基苯丙胺、氯胺酮、嗎啡、可卡因、杜冷丁、海洛因、美沙酮、地西泮、艾司唑侖九種純度標準物質(zhì)的定值工作。毒品樣品的主成分通過紅外光譜、質(zhì)譜和熔點法對其進行定性分析,純度定值分析方法則采用色譜法(液相和氣相)及差示掃描量熱法等手段,同時完成水分、無機離子和灰分含量的測定,隨機抽樣檢驗毒品樣品的均勻性、穩(wěn)定性,計算總的不確定度。結(jié)果表明九種毒品樣品的主成分與相應(yīng)標準物質(zhì)相符,定值方法測得的純品樣品純度都在99%以上,瓶間和瓶內(nèi)的均勻性良好,穩(wěn)定期在1年以上。毒品標準物質(zhì)定值建立了毒品成分量的測量方法以及相應(yīng)的國家標準物質(zhì),一方面為法庭科學(xué)領(lǐng)域的量刑等服務(wù),另一方面提高了我國法庭科學(xué)領(lǐng)域毒品成分測量在國際上的地位,使其測量結(jié)果能夠得到國際的認可,為我國在國際上相關(guān)領(lǐng)域的糾紛提供了技術(shù)支撐。 蜂蜜作為具有較高營養(yǎng)價值的天然產(chǎn)品廣泛被社會大眾所認可,但是蜂蜜中5-羥甲基糠醛的產(chǎn)生對人體有一定的危害作用。為了控制蜂蜜的質(zhì)量和保障人類身體健康,本文對蜂蜜中5-HMF基體標準物質(zhì)的定值過程進行了研究。由于蜂蜜基體的復(fù)雜性,對樣品前處理方法進行了分析研究,選擇Strata-X反相聚合物吸附劑萃取柱對樣品進行固相萃取,方法回收率在98.8%-100.5%范圍內(nèi)。采用高效液相色譜法(外標法)和同位素稀釋質(zhì)譜法(內(nèi)標法)兩種方法同時對蜂蜜中低、中、高濃度的5-HMF含量進行定值分析,濃度分別為10.8μg/g、26.9μg/g和66.4μg/g,按照國家標準物質(zhì)規(guī)范要求檢驗蜂蜜樣品的均勻性良好,穩(wěn)定期至少半年,同時進行不確定度評定。蜂蜜中5-羥甲基糠醛基體標準物質(zhì)的定值,為蜂產(chǎn)品行業(yè)的食品質(zhì)量安全提供了可靠的技術(shù)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.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2012
【分類號】：R155.5;S896.1

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