發(fā)布時(shí)間：2019-06-15 06:06

【摘要】：食品的安全問題是關(guān)乎人的生命健康的重大問題,它依賴于從生產(chǎn)源頭到銷售的各個(gè)環(huán)節(jié)。不僅需要相關(guān)的法律來規(guī)范食品的生產(chǎn)、運(yùn)輸和銷售等方面,而且還需不斷提高分析手段來控制食物的品質(zhì)。在動(dòng)物源食品的獸藥殘留分析中,復(fù)雜樣品基質(zhì)帶來的干擾是面臨的主要難題,開發(fā)具有良好生物相容性樣品前處理技術(shù)是獸藥殘留分析工作的關(guān)鍵。本實(shí)驗(yàn)采用改性的固相萃取柱對(duì)豬肉樣品中的鹽酸克倫特羅進(jìn)行了提取,并用HPLC法分離檢測(cè)。具體研究?jī)?nèi)容分為兩個(gè)部分。第一部分SDS改性固相萃取柱-HPLC法測(cè)定豬肉中的鹽酸克倫特羅目的:簡(jiǎn)化樣品前處理步驟,實(shí)現(xiàn)從豬肉的酸性勻漿液中直接提取克倫特羅,并用HPLC分離檢測(cè)。方法:采用經(jīng)表面活性劑SDS動(dòng)態(tài)改性的C18固相萃取柱,富集凈化豬肉樣品中的鹽酸克倫特羅,再經(jīng)HPLC分離檢測(cè)。結(jié)果:該方法在0.1~10.0mg/kg濃度范圍內(nèi)具有良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9989;3個(gè)濃度水平的方法回收率在96.36%~103.96%之間,RSD(n=5)在4.46%~5.10%范圍內(nèi);檢測(cè)限(S/N=3)為20.0μg/kg。結(jié)論:本實(shí)驗(yàn)所建立的方法具有快速、簡(jiǎn)便、準(zhǔn)確等特點(diǎn),成功用于動(dòng)物源食品中鹽酸克倫特羅的選擇性富集凈化和分離檢測(cè),并且有望用于其它含有疏水母核的堿性獸藥的提取分析。第二部分Tween-20改性固相萃取柱-HPLC法測(cè)定豬肉中的鹽酸克倫特羅目的:從動(dòng)物源食品中有效萃取克倫特羅的同時(shí),能顯著降低動(dòng)物食品樣品基質(zhì)中蛋白質(zhì)等大分子帶來的干擾和污染。方法:采用一定量的非離子型中性表面活性劑Tween-20對(duì)C18固相萃取柱進(jìn)行動(dòng)態(tài)改性,形成親水性表面,富集凈化豬肉中的克倫特羅,再經(jīng)HPLC分離檢測(cè)豬肉樣品中的鹽酸克侖特羅。結(jié)果:分析結(jié)果表明,該方法在0.2~10.0mg/kg添加濃度內(nèi)呈良好的線性關(guān)系,相關(guān)系數(shù)R2=0.9986;3個(gè)添加濃度(5.0mg/kg,1.0mg/kg,0.5mg/kg)回收率在96.07%~107.75%之間;RSD(n=5)在2.27%~3.51%之間;檢測(cè)限(S/N=3)為25.0μg/kg。結(jié)論:本實(shí)驗(yàn)經(jīng)非離子型中性表面活性劑Tween-20動(dòng)態(tài)改性的C18固相萃取柱,具有良好的表面親水性,對(duì)蛋白質(zhì)等大分子具有屏蔽和排阻作用,可以降低復(fù)雜基質(zhì)帶來干擾,并有效地富集凈化鹽酸克侖特羅。這是一種生物相容性固相萃取技術(shù),具有簡(jiǎn)便、高效和成本低等特點(diǎn),可廣泛應(yīng)用于動(dòng)物源食品中的獸藥殘留分析。
[Abstract]:Food safety is a major issue related to human life and health, which depends on every link from the source of production to the sale. Not only the relevant laws are needed to regulate the production, transportation and sale of food, but also analytical methods are needed to control the quality of food. In the analysis of veterinary drug residues in animal food, the interference caused by complex sample matrix is the main problem. The development of pretreatment technology of samples with good biocompatibility is the key to the analysis of veterinary drug residues. In this experiment, clenbuterol hydrochloric acid in pork samples was extracted by modified solid phase extraction column and separated and detected by HPLC. The specific research content is divided into two parts. Part 1 determination of Clenbuterol Hydrochloride in Pork by SDS modified solid Phase extraction column-HPLC objective: to simplify the pretreatment steps of samples, to extract clenbuterol directly from acid homogenate of pork, and to separate and detect clenbuterol by HPLC. Methods: C 18 solid phase extraction column modified by surfactants SDS was used to enrich and purify clenbuterol hydrochloric acid in pork samples, and then separated and detected by HPLC. Results: the method had a good linear relationship in the range of 0.1~10.0mg/kg concentration. The recovery of the method was 96.36% 鈮，

本文編號(hào)：2500020