高效液相色谱-离子阱质谱检测火锅底料中的苏丹染料Ⅰ、Ⅱ、Ⅲ、Ⅳ  

Detection of sudan dyes in hot pot dish by HPLC-ION TRAP MS/MS

作　　者：赵舰[1] 甘源[1] 张学煃[1] 

机构地区：[1]重庆市疾病预防控制中心,重庆400042

出　　处：《中国卫生检验杂志》2007年第11期1931-1933,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：用高效液相色谱/离子阱质谱仪（HPLC/ION-TRAP-MS/MS）鉴定和检测火锅底料中苏丹染料Ⅰ、Ⅱ、Ⅲ、Ⅳ。方法：样品经正己烷提取,中性氧化铝柱净化,用正己烷洗去脂肪后,再用二氯甲烷洗下苏丹染料,经浓缩至干,用甲醇溶解并定容,用ZORBAX Eclipse ODS C18柱（150 mm×2.1 mm;5μm）分离,LC-ION-TRAP-MS检测。此方法能同时鉴定和检测苏丹Ⅰ、Ⅱ、Ⅲ、Ⅳ。将已用HPLC法测定过的20件可疑样品;8件已检出苏丹Ⅰ和苏丹Ⅳ的阳性样品;1件加有苏丹Ⅰ和苏丹Ⅳ的加标样用该方法检测。结果：可疑样中有5件检测出苏丹Ⅰ和Ⅳ;阳性样中有2件仅检出苏丹Ⅳ而无苏丹Ⅰ,其余6件同HPLC法的检测结果;加标样中检测出的苏丹染料品种和量与加入品种和量相符。该方法的最低检出限分别为8.8×10^-10g、4.3×10^-9g、1.03×10^-9g、3.35×10^-10g,方法回收率为85%～95%,相对标准偏差RSD为4.56%～5.62%。结论：该方法灵敏、准确。Objective：To develop a method for characterizing and determining simultaneously 4 kinds of sudan dyes （i. s sudan Ⅰ, sudan Ⅱ , sudanⅢ, sudan Ⅳ） in the chafing dish foodstuffs by HPLC - ion trap ms/ms. Methods： The sample （ 5.0 g） was treated ultrasonically for 5 min after shaked with 30 ml hexane for 10 min,then stand. The mixture was filtered and condensed with A1203 column and the Agilent ZORBAX Eclipes ODS C17 （ 150 mm ×2. 1 mm;5 μm） was used as chromatographic column for the separation of the four dyes. A methanol and B - 1% water solution of methanoic acid was used as mobile phase at a flow rate of 0. 4 ml/min grads elution and ESI -ion trap MS spectrometer（ Finnige. Co）were used in the analysis. The quasi -molecule ion [ M ＋ H]^＋ of the 4 dyes compounds having m/z249 ,m/z277 ,m/z353 ,and m/z381 were taken as the reference ion of the given ms condition according to the time of peak appearance of these compunds,respectively. Results： Detection limit of four dyes ： sudan Ⅰ 8. 8 × 10^-10 g,sudanⅡ 4. 3 × 10^-9 g,sudanⅢ 1.03 × 10^-9 g,sudaniV 3.35 × 10^-10 g respectively. The rates of recovery were in the range from 85% to 95% ,the RSD was in the range from 4. 56% to 5.62%. Conclusion：The method is sensitive and precise for the detection of four dyes in the chafing dish.

关 键 词：HPLC/ION-TRAP-MS/MS 火锅底料 苏丹Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅳ 

分 类 号：R155.55[医药卫生—营养与食品卫生学]