HPLCMS/MS Determination of Na2EDTA in Food
标 签 高效液相色谱串联质谱法 食品 乙二胺四乙酸二钠 HPLCMS/MS Food Na2 EDTA
应用高效液相色谱串联质谱法(HPLCMS/MS)测定了食品中EDTA二钠盐。液态食品(5 g)直接加水40 mL提取;固态或酱状食品(5 g)加水15 mL及三氯甲烷20 mL匀质后离心,取其上清液,残渣重复提取2次。合并上清液,在提取液中加入三氯化铁溶液超声10 min衍生化后,定容至50 mL。取样品溶液5 mL,经MAX阴离子交换柱净化,用甲酸甲醇水(10+50+40)混合液6 mL洗脱,洗脱液经80 ℃吹氮蒸干,用水溶解后进行HPLCMS/MS分析。EDTA二钠盐的质量浓度在1.0~50.0 mg·L-1范围内呈线性。方法的检出限(3S/N)为5 mg·kg-1。应用提出的方法分析了4种食品样品并进行加标回收试验,测得回收率在88.3%~96.0%之间,测定值的相对标准偏差(n=6)均小于10%。
HPLCMS/MS was applied to the determination of Na2EDTA in food. Na2EDTA in liquid samples (5 g) was extracted directly with 40 mL of water; while in solid or jam samples, was extracted by mixing and centrifuging with 15 mL of H2O and 20 mL of CHCl3, the supernatant was collected, and the lower phase was reextracted twice, the supernatants were collected and combined. The combined extract was then derivatized with FeCl3 solution by mixing ultrasonically for 10 min, and the mixture was made up to 50 mL. An aliquot of 5 mL of the derivatized solution was taken and purified by passing through MAX SPE column. The column was eluted with 6 mL of a mixture of HCOOHCH3OHH2O (10+50+40). The eluate was evaporated to dryness by N2blowing at 80 ℃, and the residue was dissolved with water. This solution was used for HPLCMS/MS analysis. Linearity range was found between 1.0-50.0 mg·L-1 for Na2EDTA. Detection limit (3S/N) found was 5 mg·kg-1. Four samples were analyzed by this method and test for recovery was made by standard addition method. Values of recovery obtained were in the range of 88.3%-96.0%, with RSD′s (n=6) all less than 10%.
引用该论文: WEI Dongxu,HAN Guangyuan,SUN Ying,HU Shaoxin,YANG Changzhi. HPLCMS/MS Determination of Na2EDTA in Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(6): 698～701
魏冬旭,韩广源,孙莹,胡少新,杨长志. 高效液相色谱-串联质谱法测定食品中的乙二胺四乙酸二钠[J]. 理化检验－化学分册, 2014, 50(6): 698～701