色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
1期
80-83
,共4页
曾琪%张缙%徐敦明%张志刚%柯志成
曾琪%張縉%徐敦明%張誌剛%柯誌成
증기%장진%서돈명%장지강%가지성
高效液相色谱%荧光检测%尿素%罐头食品%呫吨醇
高效液相色譜%熒光檢測%尿素%罐頭食品%呫噸醇
고효액상색보%형광검측%뇨소%관두식품%첩둔순
high performance liquid chromatography( HPLC)%fluorescence detection( FLD)%urea%canned food%xanthydrol
建立了罐头食品中尿素残留检测的柱前衍生-高效液相色谱-荧光检测方法。取5.0 g样品,经20 mL 1%( v/v)乙酸溶液提取、定容,离心后取上清液过滤,吸取0.5 mL 提取液用呫吨醇进行衍生,采用高效液相色谱-荧光检测器进行测定。尿素在0.1~500 mg/L内线性良好,相关系数大于0.9995。实验表明,在5种罐头食品中各添加0.001~30 g/kg 尿素,其平均回收率为80.2%~109.7%,相对标准偏差( n=6)为2.05%~6.53%,检出限为0.5 mg/kg,定量限为1.0 mg/kg。利用本研究建立的方法对168个实际样品进行测定,在3个肉类罐头样品中检出尿素,含量分别为10.6、62.1和2.6 mg/kg。方法稳定、可靠、操作简单,适用于罐头食品中尿素的检测。
建立瞭罐頭食品中尿素殘留檢測的柱前衍生-高效液相色譜-熒光檢測方法。取5.0 g樣品,經20 mL 1%( v/v)乙痠溶液提取、定容,離心後取上清液過濾,吸取0.5 mL 提取液用呫噸醇進行衍生,採用高效液相色譜-熒光檢測器進行測定。尿素在0.1~500 mg/L內線性良好,相關繫數大于0.9995。實驗錶明,在5種罐頭食品中各添加0.001~30 g/kg 尿素,其平均迴收率為80.2%~109.7%,相對標準偏差( n=6)為2.05%~6.53%,檢齣限為0.5 mg/kg,定量限為1.0 mg/kg。利用本研究建立的方法對168箇實際樣品進行測定,在3箇肉類罐頭樣品中檢齣尿素,含量分彆為10.6、62.1和2.6 mg/kg。方法穩定、可靠、操作簡單,適用于罐頭食品中尿素的檢測。
건립료관두식품중뇨소잔류검측적주전연생-고효액상색보-형광검측방법。취5.0 g양품,경20 mL 1%( v/v)을산용액제취、정용,리심후취상청액과려,흡취0.5 mL 제취액용첩둔순진행연생,채용고효액상색보-형광검측기진행측정。뇨소재0.1~500 mg/L내선성량호,상관계수대우0.9995。실험표명,재5충관두식품중각첨가0.001~30 g/kg 뇨소,기평균회수솔위80.2%~109.7%,상대표준편차( n=6)위2.05%~6.53%,검출한위0.5 mg/kg,정량한위1.0 mg/kg。이용본연구건립적방법대168개실제양품진행측정,재3개육류관두양품중검출뇨소,함량분별위10.6、62.1화2.6 mg/kg。방법은정、가고、조작간단,괄용우관두식품중뇨소적검측。
A method for the determination of urea residue in canned foods by high performance liquid chromatography-fluorescence detection( HPLC-FLD)coupled with precolumn derivatiza-tion was established. The sample(5. 0 g),including canned edible fungi,fruit,vegetable,fish, and meat was extracted with 20 mL 1%( v/v)acetic acid solution. The extract was centrifuged, filtrated,and then derivatized with xanthydrol. The analysis was completed with HPLC-FLD. A good linear relationship was obtained in the range of 0. 1-500 mg/L with the correlation coeffi-cients more than 0. 999 5. The average recoveries of urea spiked at 0. 001-30 g/kg levels in five kinds of canned foods ranged from 80. 2% to 109. 7% with the RSDs of 2. 05%-6. 53%. The limit of detection(LOD)was 0. 5 mg/kg,and the limit of quantitation(LOQ)was 1. 0 mg/kg. The proposed procedure was then applied to the analysis of 168 real samples collected from Xia-men,Fujian Province,China. The existence of urea was found in three pork cans with contents of 10. 6,62. 1 and 2. 6 mg/kg,respectively. The method is stable,reliable,simple and suitable for the determination of urea in canned foods,and has great potential for routine analysis in foodstuffs.