氣相色譜—質(zhì)譜聯(lián)用技術(shù)測(cè)定食品中鄰苯二甲酸酯類的研究
本文選題:鄰苯二甲酸酯 + 氣相色譜-質(zhì)譜聯(lián)用儀 ; 參考:《河南大學(xué)》2013年碩士論文
【摘要】:鄰苯二甲酸酯類化合物是一類重要的增塑劑,被廣泛用于塑料制品的生產(chǎn),在其他鄰域也有應(yīng)用,,例如化妝品、香精等的生產(chǎn)。鄰苯二甲酸酯也是環(huán)境激素的一種,而環(huán)境激素是一類可以對(duì)人體產(chǎn)生有害影響的物質(zhì)。隨著塑料制品的大量使用使環(huán)境中的鄰苯二甲酸酯含量不斷增加,而環(huán)境中的鄰苯二甲酸酯也會(huì)遷移進(jìn)入食物,進(jìn)而進(jìn)入人體,危害人體健康。雖然,鄰苯二甲酸酯有降解途徑,但其降解非常緩慢,因而,減少塑料制品使用的同時(shí),建立快速、準(zhǔn)確、安全的測(cè)定分析法是很必要和必須的。 本文選定被廣泛關(guān)注的16種鄰苯二甲酸酯類增塑劑(鄰苯二甲酸二甲酯(DMP)、鄰苯二甲酸二乙酯(DEP)、鄰苯二甲酸二異丁酯(DIBP)、鄰苯二甲酸二丁酯(DBP)、鄰苯二甲酸(2-甲氧基)乙酯(BMEP)、鄰苯二甲酸二(4-甲基-2-戊基)(BMPP)、鄰苯二甲酸二(2-乙氧基)乙酯(BEEP)、鄰苯二甲酸二戊酯(DPP)、鄰苯二甲酸二己酯(DHXP)、鄰苯二甲酸丁基芐基酯(BBP)、鄰苯二甲酸己酯2-乙基己基酯(HEP)、鄰苯二甲酸二(2-丁氧基)乙酯(BnBP)、鄰苯二甲酸二環(huán)己酯(DCHP)、鄰苯二甲酸二(2-乙基)己酯(DEHP)、鄰苯二甲酸二丁正辛酯(DOP)和鄰苯二甲酸二壬酯(DNP))作為研究對(duì)象,選擇DB-5MS毛細(xì)管色譜柱,確定進(jìn)樣口溫度,選擇離子檢測(cè)(SIM)定性,使用氣相色譜-質(zhì)譜聯(lián)用儀(GC-MS)進(jìn)行分析,經(jīng)過試驗(yàn)系統(tǒng)研究并建立了16種鄰苯二甲酸酯類污染物的分析方法,確定了線性范圍、線性相關(guān)性以及最低檢出限,很好地滿足了分析檢測(cè)鄰苯二甲酸酯類化合物的需要。 以食用油、液態(tài)奶、葉類蔬菜為材料,優(yōu)化了前處理方法。食用油經(jīng)乙腈提取SILICA/PSA玻璃混合型固相萃取柱凈化,回收率在80.0%~105.0%,相對(duì)標(biāo)準(zhǔn)偏差(n=6)在2.7%~5.7%之間,結(jié)果表明該分析方法準(zhǔn)確度、精密度良好;液態(tài)奶和葉類蔬菜分別進(jìn)行了不同有機(jī)溶劑提取試驗(yàn),確定提取溶劑正己烷、乙醚、乙腈的提取比例。結(jié)果表明鄰苯二甲酸酯類化合物在液態(tài)奶中的回收率為80.0%~104.0%,相對(duì)標(biāo)準(zhǔn)偏差(n=6)為2.1%~5.1%,葉類蔬菜樣品中的回收率為75.4%~110.6%,相對(duì)標(biāo)準(zhǔn)偏差(n=6)為3.8%~12.4%。
[Abstract]:Phthalic acid esters are important plasticizers, which are widely used in the production of plastic products, and are also used in other neighborhoods, such as cosmetics, flavor and so on. Phthalate is also a kind of environmental hormone, which can have harmful effects on human body. With the extensive use of plastic products, the content of phthalate in the environment is increasing, and the phthalate in the environment will migrate into food, and then into the human body, which is harmful to human health. Although phthalate has a degradation pathway, its degradation is very slow. Therefore, it is necessary and necessary to establish a rapid, accurate and safe analytical method while reducing the use of plastic products. In this paper, 16 kinds of phthalate plasticizers (dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate, dimethoxy phthalate, dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, dibutyl phthalate, dimethoxy phthalate) have been selected. BMEPN, Ding Ji benzyl phthalate, 2-ethylhexyl phthalate, dimethyl phthalate 2-ethoxy, dipentyl phthalate, dihexyl phthalate, Ding Ji benzyl phthalate, 2-ethylhexyl phthalate, benzyl phthalate, 2-ethylhexane phthalate, dipentyl phthalate, dihexyl phthalate, benzyl phthalate, hexyl phthalate, diethyl hexane phthalate, dipentyl phthalate, dihexyl phthalate. Hep, BnBPN, DCHPU, DEHPN, DOP) and DNPN) were used as the research objects, and the results were as follows: (1) Ester (Hep), (dibutoxy phthalate) ethyl (BnBPN), DHPX (dicyclohexyl phthalate), (dibutylhexyl phthalate) (DOP) and DNPN (DNPN) were used as the objects of the study. The DB-5MS capillary column was selected, the injection temperature was determined, and the qualitative analysis was carried out by ion detection (Simm). The analytical method of 16 phthalate esters was established by gas chromatography-mass spectrometry (GC-MS). The linear range, the linear correlation and the minimum detection limit were determined, which satisfied the needs of analysis and detection of phthalates. Using edible oil, liquid milk and leafy vegetables as materials, the pretreatment method was optimized. The purification of edible oil by acetonitrile SILICA/PSA glass mixed solid phase extraction column showed that the recovery rate was 80. 0% and the relative standard deviation was 2. 757%. The results showed that the method was accurate and accurate. The extraction ratio of n-hexane, ether and acetonitrile in liquid milk and leaf vegetables were determined by different organic solvents. The results showed that the recovery rate of phthalates in liquid milk was 80. 0 and 10. 0, and the relative standard deviation was 2. 1 and 5. 1. The recovery rate in leaf vegetables was 75. 4% and 110.6, and the relative standard deviation was 3. 8 and 12. 4, respectively.
【學(xué)位授予單位】:河南大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2013
【分類號(hào)】:O657.63;R155.51
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