時(shí)小艷



摘要:建立一種采用高效液相色譜法(HPLC)測定加工肉制品中吲哚殘留量的新方法。樣品經(jīng)純甲醇提取后,采用HLB固相萃取柱凈化,用高效液相色譜C18柱分離,水-乙腈作為流動(dòng)相,流速為1.0 mL/min,柱溫為30 ℃,紫外檢測波長為275 nm,外標(biāo)法定量。吲哚的濃度在10~100 μg/L內(nèi)有較好的線性關(guān)系,R2大于0.99,回收率為93.5%~97.4%,RSD小于15%(n=10)。該法簡單,靈敏度高,重復(fù)性好,適用于動(dòng)物源性食品中吲哚殘留量的測定。
關(guān)鍵詞: 吲哚; 高效液相色譜; 殘留
中圖分類號(hào):O657.7+2 ? ? ? ?文獻(xiàn)標(biāo)識(shí)碼:A ? ? ? ?文章編號(hào):0439-8114(2015)23-6015-03
DOI:10.14088/j.cnki.issn0439-8114.2015.23.056
Content Determination of Indole in Meat Products Processing by HPLC
SHI Xiao-yan
(Department of Career Technical, Jiangsu Food and Drug of Medicine and Health Management College, Huaian 223003, Jiangsu, China)
Abstract: To establish a high performance liquid chromatography (HPLC) method for determination of indole residues in meat food, samples were extracted with methanol, purified with HLB solid phase extraction column, separated by C18 chromatography column. Water-acetonitrile was acted as the mobile phase with gradient elution, the flow rate was 1.0 mL/min, column temperature was 30 ℃,the detection wavelength was 275 nm with external standard method. Indole concentration in 10~100 g/L had good linear relationship, regression coefficient was more than 0.99, the recoveries were in the range of 93.5%~97.4%,the relative standard deviation was less than 15%(n=10). The method was simple, rapid, sensitive, suitable for determination of indole residues in animal origin food.
Key words:indole;high performance liquid chromatography;residues
吲哚是吡咯與苯并聯(lián)的化合物,又稱苯并吡咯,結(jié)構(gòu)如圖1所示。熔點(diǎn)在51~54 ℃之間,密度為1.14 g/cm3[1]。吲哚及其同系物和衍生物廣泛存在于自然界中,主要存在于天然花油中,如茉莉花、水仙花、香羅蘭等中。吲哚是一種重要的有機(jī)原料和精細(xì)化工產(chǎn)品,是動(dòng)物必需氨基酸色氨酸的衍生物,植物生長素(吲哚-3-乙酸)、抗炎藥物消炎痛、生物堿及色素中也包含有吲哚結(jié)構(gòu)。由于吲哚在化工中被廣泛應(yīng)用,必須控制在允許范圍內(nèi),避免對(duì)人體健康帶來威脅[2-4]。
高效液相色譜法以液體為流動(dòng)相,采用高壓輸液系統(tǒng),將具有不同極性的單一溶劑或不同比例的混合溶劑、緩沖液等流動(dòng)相泵入裝有固定相的色譜柱,在柱內(nèi)各成分被分離后,進(jìn)入檢測器進(jìn)行檢測,從而實(shí)現(xiàn)對(duì)試樣的分析。該方法已成為化學(xué)、醫(yī)學(xué)、工業(yè)、農(nóng)學(xué)、商檢和法檢等學(xué)科領(lǐng)域中重要的分離分析技術(shù)[5-7]。本試驗(yàn)通過高效液相色譜來測定肉制品中吲哚的含量,該方法簡單、可操作性強(qiáng),靈敏度高。……