6 11 Vol. 6 No. 11 2015 11 Journal of Food Safety and Quality Nov., 2015 - 马灵飞 1 1,, 周围 2, 张雅珩 2, 周小平 (1., 730070; 2., 730010) 1, 2* 摘要 : 目的 - (HS-GC) 方法 N,N- (DMF),, 结果,, 1.50 mg/kg, 1.84%, 96% 113% 结论, 关键词 : - ; ; Determination of solvent-extracted oil No.6 in sun flower seed meal by head-space gas chromatography MA Ling-Fei 1, ZHOU Wei 1, 2, ZHANG Ya-Heng 2 1, 2*, ZHOU Xiao-Ping (1. College of Geography and Environmental Science, Northwest Normal University, Lanzhou 730070, China; 2. Central Laboratory of Technical Center of Gansu Entry-Exit Inspection and Quarantine Bureau, Lanzhou 730010, China) ABSTRACT: Objective To establish a new method for the determination of solvent-extracted oil No.6 in sun flower seed meal by head-space gas chromatography (HS-GC). Methods Samples of sunflower seed meal were soaked in N,N-dimethylformamide, and the qualitative and quantitative analysis was used by HS-GC. The experiment conditions were optimized. The sample preprocessing method conditions, the equilibrium temperature and time of headspace automatic sampler, the column temperature and the split ratio were all determined. Results The components of solvent-extracted oil No.6 were separated from each other completely. The method had a good linearity. The detection limit of the method could reach 1.50 mg/kg, with the accuracy of 1.84%, and the recovery of solvent-extracted oil No.6 was in the range of 96%~113%. Conclusion The method is simple, rapid and reproducible, which can provide a reliable method for the determination of residual solvents in sunflower seed meal. KEY WORDS: head-space gas chromatography; solvent-extracted oil No.6; sun flower seed meal 1 引言,, 1.1% 4.5%, 29% 43%,,,, [1,2],,, * 通讯作者 :,,, E-mail: zhxp1123@163.com *Corresponding author: ZHOU Xiao-Ping, Senior Engineer, College of Geography and Environmental Science, Northwest Normal University, Central Laboratory of Technical Center of Gansu Entry-Exit Inspection and Quarantine Bureau, Lanzhou 730020, China. E-mail: zhxp1123@163.com
11, : - 4423, [3],, [4,5],,, -,,,,,, [6-8],, - [9], [10], [3] 3,, -, 2 材料与方法 2.1 材料与试剂 :,,, 60 : N,N- (DMF), ( ) : (10 mg/ml), N,N-, 2.2 仪器 Clarus600 ( PerkinElmer ), (FID); AutoHS ( ); 20 ml ; 2.3 顶空条件 : 120 s; : 2 s; : 20 s; : 20 min; : 16 min; : 70 ; 105 ; 105 ; : 67 kpa 2.4 色谱条件 : HP-5MS (30 m 0.32 mm, 0.25 μm); 5.5 psi; 50 10 min; : 200 ; : ; : 100:1; : 200 ; : N 2 ( 99.99%) ; H 2 : 45 ml/min, : 450 ml/min 2.5 标准曲线的绘制 DMF 5.0 10.0 15.0 20.0 30.0 μg/ml 10.0 ml, 20 ml, 2.3, 2.4, 2.6 样品测定 1.00 g 20 ml, 10.00 ml DMF,,, 2.3 2.4 2.7 加标样品的测定 1.00 g 20 ml, 1 μl, 10.00 ml DMF,,, 2.3 2.4 2.8 实验条件的优化 2.8.1 前处理条件的优化, 2.6, 2.3 2.4 : ; : DMF, DMF, DMF DMF 2.8.2 气相色谱条件的优化 (40 200 ),, 2.3 2.4, 2.3 2.4, (100:1 20:1) 2.8.3 顶空条件的优化 2.7, 40 50 60 70 80 90,
4424 6 2.3, 2.4, 0 20 30 40 50 60 min, 2.7, 2.3 2.4, 3 结果与分析 3.1 前处理条件的优化 3, 2.8, 2.6,,, ;,, 2.6 3.2 气相色谱条件的优化,, : 50 (100:1 20:1), : 100:1,, 1 3.3 顶空条件的优化,, [12-14] 3.3.1 平衡时间的优化 60, 10 20 30 40 50 60 min, 2.7 2 : 10~50 min,, 60 min, 20 min 20 min 3.3.2 平衡温度的优化 60, 40 50 60 70 80 90, 2.7 3 ;, 70,,, 70 Fig. 1 1 Chromatogram of solvent-extracted oil No.6 in sunflower seed meal
11, : - 4425,, (n=6), 1 2 Fig. 2 Effect of equilibrium time on peak area 4 6 Fig. 4 Standard curve of solvent-extracted oil No.6 Fig. 3 3.4 方法评价 3 Effect of equilibrium temperature on peak area 3.4.1 方法线性范围和检出限 2.5, 4; 3.4.2 方法的回收率 5 1.00 g, 0.0 10.0 15.0 20.0 30.0 μg, 2,, 2 3.5 实际样品的测定 -, 5, 3 表 1 检出限和回归方程的测定结果 Table 1 Testing results of regression equations and detection limit (mg/kg) (n=6,%) Y=259.85X+480.95 0.9986 1.50 1.84 表 2 回收率测定结果 Table 2 Testing results of recovery rate (mg/kg) (%) (n=2,%) (%) 99.8 10 108.3 5.78 104.0 109.4 15 2.41 111.3 113.2 102.5 20 3.17 104.8 107.2 94.1 30 97.9 2.80 96.0
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