7 7 Vol. 7 No. 7 2016 7 Journal of Food Safety and Quality Jul., 2016 - 王 绍 青 1, 高 洁 2, 周 宇 1, 徐 雯 雯 1, 朱 莉 萍 (1., 272067; 2., 272000) 2* 摘 要 : 目 的 - (inductively coupled plasma-mass spectrometry, ICP-MS) (Cr) (As) (Cd) 方 法, ICP-MS Cr As Cd ; GB 5009-2014, 结 果 1 5 10 μg/kg 3, 96.1%~104.7 %, 5.52% Cr As Cd 0~50 μg/kg, r 0.99 34.78~131.67 μg/kg, 8.33~21.76 μg/kg, 11.42~21.52 μg/kg, 结 论, 关 键 词 : ; ; ; ; Rapid detection of heavy metals in instant noodles by microwave digestioninductively coupled plasma-mass spectrometry WANG Shao-Qing 1, GAO Jie 2, ZHOU Yu 1, XU Wen-Wen 1, ZHU Li-Ping 2* (1. School of Public Heath, Jining Medical University, Jining 272067, China; 2. Jining Entry-Exit Inspection and Quarantine Bureau, Jining 272000, China) ABSTRACT: Objective To establish a method for determination of heavy metals including Cr, As and Cd in instant noodles by inductively coupled plasma-mass spectrometry (ICP-MS) with microwave digestion pretreatment. Methods Instant noodle samples were digested by microwave and then detected by ICP-MS for measurement of the content of Cr, As and Cd. At the same time, the method was compared with GB 5009-2014 to verify the feasibility and the content of heavy metals (Cr, As, Cd) in instant noodles sold in Jining city was detected. Results The recoveries spiked at 3 levels of 1, 5 and 10 μg/kg were 96.1%~104.7% with RSDs less than 5.52%. Cr, As, and Cd had good linear relationships in 0~50 μg/kg with coefficient correlations larger than 0.99. The content of Cr in instant noodle were in the range of 34.78~131.67 μg/kg, the content of As were in the range of 8.33~21.76 μg/kg and the content of Cd were in the range of 11.42~21.52 μg/kg, all of them did not exceed the national standards. Conclusion The method is rapid and precise, which is suitable for determination of heavy metals in instant noodles. KEY WORDS: instant noodles;inductively coupled plasma mass spectrometry; Cr; As; Cd * 通 讯 作 者 :,, E-mail: gufeng1979@163.com *Corresponding author: ZHU Li-Ping, Engineer, Jining Entry-Exit Inspection and Quarantine Bureau, No.62 Guanghe Road, Jining 272025, China. E-mail: gufeng1979@163.com
7, : - 2799 1 引 言,, [1] [2], [3,4],,,,, [5-8],,, [9,10],,,, [11], (inductively coupled plasma-mass spectrometry, ICP-MS) [12,13] ICP-MS,, [14,15], [16] ICP-MS, ICP-MS, GB 5009.11-2014 [17] GB 5009.15-2014 [18] GB 5009.123-2014 [19],, 2 材 料 与 方 法 2.1 材 料 6, A B C D E F, 2.2 仪 器 与 试 剂 7700X - ( ); CPA225D ( Sartorius AG ); MARS.6 (, ); DV-4000 ( ANNAN ); DST-1000 ( SAVILLEX ); 613-UF-70 () 70% (, );, 18.2 MΩ cm, (Cr) (As) (Cd) 10 μg/ml, 2.3 实 验 方 法 2.3.1 试 样 前 处 理,,, 1 g ( 0.01 g), 8 ml, 1 h,,,, 160, 20 min 25 ml, 3, 25 ml,, 2.3.2 标 准 品 及 标 准 系 列 的 配 制 3 Cr As Cd : 2% 10 μg/ml 0 2 5 10 20 50 μg/kg 2.3.3 仪 器 条 件 5 min 120 ( 1 min), 3 min 155 ( 5 min), 5 min 180 ( 10 min) 2.3.4 加 标 样 品 的 配 制 3 Cr As Cd, 6,, 3 结 果 与 分 析 3.1 微 波 消 解 条 件 的 确 定,,,,, 3.1.1 消 解 温 度 选 择, 1 1, 120-155 -180 3.1.2 最 高 消 解 温 度 保 持 时 间 的 选 择 120-155 -180, 180 2, 180 10 min, 5 min 120 ( 1 min), 3 min 155 ( 5 min), 5 min 180 ( 10 min),,,
2800 7 Table 1 表 1 微 波 消 解 程 序 的 选 择 Selection of microwave digestion procedure 1( )/ (min) (min) 2( ) (min) 3( )/ (min) R(Cr)/% R(Se)/% R(Cd)/% 1 100/5 3 130 5 160/10 71 63 70 2 120/5 3 140 5 150/10 83 76 87 3 120/5 3 155 5 180/10 94 98 102 4 120/5 3 160 5 200/10 93 99 98 R Note: R stands for recovery. Table 2 表 2 最 终 温 度 保 持 时 间 的 选 择 Selection of holding time of final temperature 180 /(min) R(Cr)/% R(Se)/% R(Cd)/% 1 3 62 60 71 2 5 76 72 80 3 10 96 97 105 3.2 标 准 曲 线 方 法 检 出 限 和 精 密 度, 3 2 5 10 20 50 μg/kg, 1~3, 3, r 0.99 6, 0.79%~2.45%, 11, 3, 3 3.3 样 品 的 测 定 6 Cr As Cd 4 4, 6,, 3 GB 2762-2012 2 As Fig. 2 The standard curve of As 1 Cr Fig. 1 The standard curve of Cr 3 Cd Fig. 3 The standard curve of Cd
7, : - 2801 Table 3 表 3 标 准 曲 线 精 密 度 和 检 出 限 (n=6) Standard curves, RSDs and limits of detection (n=6) (μg/ml) RSD(%) (mg/kg) Cr 0~50 Y = 0.0876X + 0.0759 0.9986 2.45 0.01 As 0~50 Y = 0.0004X + 0.0002 0.9989 0.79 0.02 Cd 0~50 Y = 0.0008X + 0.0003 0.9993 1.28 0.01, -ICP-MS 表 4 优 化 方 法 与 国 标 方 法 测 得 C 品 牌 方 便 面 重 金 属 含 量 比 较 Table 4 Comparison of heavy metal contents of C brand instant noodles by optimized method and national standard method (μg/kg ) ( μg/kg ) Cr 34.78 32.69 Fig. 4 4 6 Cr As Cd Cr, As, and Cd content of 6 brands of instant noodles [20] (0.1 mg/kg) (0.5 mg/kg) (1.0 mg/kg),, 6 3 3.4 优 化 后 方 法 与 国 标 法 分 别 检 测 样 品 中 Cr, As, Cd 含 量 对 比 C,, 4, As 8.33 9.15 Cd 18.14 18.48 3.5 样 品 加 标 回 收 率 C, 3 Cr As Cd, 6, 2 2, 96.1%~104.7 %, 5.52%, -,, 表 5 C 品 牌 样 品 加 标 回 收 率 (n=6) Table 5 Recoveries of C brand sample (n=6) (μg/kg) (μg/kg) (%) RSD(%) (%) RSD(%) 0 1 96.1 2.52 94.7 2.10 Cr 0 5 98.9 2.70 96.0 1.56 0 10 99.3 1.16 99.7 0.66 0 5 104.7 2.58 89.6 2.02 As 0 10 102.5 2.81 88.2 2.83 0 20 98.7 2.33 94.3 1.69 0 10 97.6 2.50 100.3 2.56 Cd 0 20 98.2 0.76 92.4 2.77 0 50 97.2 1.20 97.7 1.87
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