建立了面粉及其制品中联二脲的液相色谱-串联质谱（ LC-MS/MS）测定及确证方法。采用纯水振荡提取样品中的联二脲，联二脲经高锰酸钾氧化后，转变为偶氮甲酰胺，再加入对甲苯亚磺酸钠使偶氮甲酰胺衍生为对甲苯磺酰氨基脲。以乙腈和2 mmol/L乙酸铵溶液（含0.2％（ v/v）甲酸）为流动相进行梯度洗脱，经 Shimpak XR-ODSⅡ色谱柱（150 mm×2.0 mm，2.2μm）分离，电喷雾正离子模式电离（ESI＋），多反应监测（MRM）模式检测，同位素内标法定量。方法的线性范围为1~20000μg/kg，相关系数为0.9999，定量限为5μg/kg；当添加水平为5.0、10.0与50.0μg/kg时，联二脲的平均回收率为78.3％~108.0％，相对标准偏差（ RSDs）不大于5.73％。本方法新颖、可靠、灵敏、线性范围广，而且实用性强，可用于面粉及其多种制品中联二脲的测定和确证。
A novel method was established for the determination and identification of biurea in flour and its products using liquid chromatography-tandem mass spectrometry( LC-MS/MS). The biurea was extracted with water and oxidized to azodicarbonamide by potassium permanga-nate. The azodicarbonamide was then derivatized using sodium p-toluene sulfinate solution. The separation was performed on a Shimpak XR-ODSⅡ column(150 mm×2. 0 mm,2. 2 μm)using the mobile phase composed of acetonitrile and 2 mmol/L ammonium acetate aqueous solution (containing 0. 2%(v/v)formic acid)with a gradient elution program. Tandem mass spectro-metric detection was performed in multiple reaction monitoring( MRM)scan mode with a posi-tive electrospray ionization( ESI+)source. The method used stable isotope internal standard quantitation. The calibration curve showed good linearity over the range of 1-20 000 μg/kg( R 2=0. 999 9). The limit of quantification was 5 μg/kg for biurea spiked in flour and its products. At the spiking levels of 5. 0,10. 0 and 50. 0 μg/kg in different matrices,the average recovery of biurea was 78. 3%-108. 0% with the relative standard deviations( RSDs)≤5. 73%. The method developed is novel,reliable and sensitive with wide linear range,and can be used to determine the biurea in flour and its products.
参考文献
| [1] | 吴正双;梁炽琼;钟海娟.[J].现代食品科技,201228(09):1239. |
| [2] | 龙彪;单军;杨立军.[J].食品研究与开发,201233(07):236. |
| [3] | GB2760-2011.[S]. |
| [4] | Becalski A;Lau B P Y;Lewis D.[J].Journal of Agricultural and Food Chemistry,200452(18):5730. |
| [5] | Noonan G O;Begley T H;Diachenko G W.[J].Journal of Agricultural and Food Chemistry,200856(06):2064. |
| [6] | Becalski A;Lau B P Y;Lewis D.[J].Food Additives and Contaminants,200623(02):107. |
| [7] | Noonan G O;Warner C R;Hsu W.[J].Journal of Agricultural and Food Chemistry,200553(12):4680. |
| [8] | 赵晓燕;潘明旺;袁金凤.[J].河北工业大学学报,201039(03):29. |
| [9] | Bechtold W E;Shopp G M;Cheng Y S.[J].Journal of Analytical Toxicology,198812(02):89. |
| [10] | Mulder P P J;Beumer B;Van Rhijn J A.[J].Analytica Chimica Acta,2007586(1/2):366. |
| [11] | 袁丽红;丁洪流;陈英.[J].食品工业科技,201334(10):73. |
| [12] | Bechtold W E;Medinsky M A;Cheng Y S.[J].Xenobioti-ca,198919(09):1003. |
| [13] | Hunter B A .[P].United States Patent,3903157,1975-09-02. |
| [14] | Ye J;Wang X H;Sang Y X.[J].Journal of Agricultural and Food Chemistry,201159(17):9313. |
| [15] | Lozano A;Rajski L;Belmonte-Valles N.[J].J Chroma-togr A,20121268:109. |
| [16] | 贾彦波;王清清;宋海峰.[J].军事医学,201135(02):149. |
| [17] | 严爱花;李贤良;郗存显.[J].分析化学,201341(04):509. |
| [18] | 杨涛;王静静;鹿毅.[J].广州化工,201341(12):150. |
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