Microsoft Word 王绍青二校

Size: px

Start display at page:

Download "Microsoft Word - 2798-2802 20160520003王绍青二校"

梯卢燕
7 years ago
Views:

1 7 7 Vol. 7 No Journal of Food Safety and Quality Jul., 王绍青 1, 高洁 2, 周宇 1, 徐雯雯 1, 朱莉萍 (1., ; 2., ) 2* 摘要 : 目的 - (inductively coupled plasma-mass spectrometry, ICP-MS) (Cr) (As) (Cd) 方法, ICP-MS Cr As Cd ; GB , 结果 μg/kg 3, 96.1%~104.7 %, 5.52% Cr As Cd 0~50 μg/kg, r ~ 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 , China; 2. Jining Entry-Exit Inspection and Quarantine Bureau, Jining , 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 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 The content of Cr in instant noodle were in the range of 34.78~ 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 :,, gufeng1979@163.com *Corresponding author: ZHU Li-Ping, Engineer, Jining Entry-Exit Inspection and Quarantine Bureau, No.62 Guanghe Road, Jining , China. gufeng1979@163.com

99 34.78~131.67 μg/kg, 8.33~21.76 μg/kg, 11.42~21.

2 7, : 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 [17] GB [18] GB [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 实验方法试样前处理,,, 1 g ( 0.01 g), 8 ml, 1 h,,,, 160, 20 min 25 ml, 3, 25 ml,, 标准品及标准系列的配制 3 Cr As Cd : 2% 10 μg/ml μg/kg 仪器条件 5 min 120 ( 1 min), 3 min 155 ( 5 min), 5 min 180 ( 10 min) 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,,,,, 消解温度选择, 1 1, 最高消解温度保持时间的选择 , 180 2, min, 5 min 120 ( 1 min), 3 min 155 ( 5 min), 5 min 180 ( 10 min),,,

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.

3 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/ / / / / / / / 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)/% 标准曲线方法检出限和精密度, μg/kg, 1~3, 3, r , 0.79%~2.45%, 11, 3, 样品的测定 6 Cr As Cd 4 4, 6,, 3 GB 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

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.

4 7, : 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 = X As 0~50 Y = X Cd 0~50 Y = X , -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 Fig 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),, 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 Cd 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(%) Cr As Cd

5 结论,,,, ICP-MS,,,, 6 Cr As Cd, GB [21] GB [20] 参考文献 [1],,,. [J]., 2016, 42(4): Li L, Tan L, Duan LP, et al. Progress of the sources of heavy metal pollution in food [J]. Food Ferment Ind, 2016, 42(4): [2] Zhang ZW, Watanabe T, Shimbo S, et al. Lead and cadmium contents in ceress and pulses in north-eastern China [J]. Sci Total Environ, 1998, 220(2 3): [3] Liu XM, Song QJ, Tang Y, et al. Human health risk assessment of heavy metals in soil-vegetable system: A multi-medium analysis [J]. Sci Total Environ, 2013, c(5): [4] Nesterkova V, Vorobeichike L, R eznichenkoi S. The effect of heavy metals on the soil-earthworm-europena mole food chain under the conditions of environmental pollution caused by the emissions of a copper smelting plant [J]. Contemp Probl Ecol, 2014, 7(5): [5]. ICP-OES [J]., 2013, 34(1): Fu L. Determination of trace elements in instant noodles by inductively coupled plasma optical emission spectrometry [J]. Food Ind, 2013, 34(1): [6],. [J]., 2013, 39(11): Xu HY, Bao YL. Determination of heavy metal elements lead and arsenic in instant noodles seasoning [J]. China Condim, 2013, 39(11): [7],,,. [J]., 2015, 6: YU SS, LI JX, RAO HJ, et al. Detection and analysis of harmful substances of instant noodles [J]. China Food Saf, 2015, 6: [8],,,. [J]., 2010, 29(11): Duan JF, Zhang XL, Shi RF, et al. The determination of acrylamide in fried instant noodles with high performance liquid chromatographic method [J]. Chin J Anal Lab, 2010, 29(11): [9] Kapungwe EM. Heavy metal contaminated food crops irrigated with wastewater in Peri urban areas, Zambia [J]. Open J Metal, 2013, 3(2): [10] Hu XF, Jiang Y, Shu Y, et al. Effects of mining wastewater discharges on heavy metal pollution and soil enzyme activity of the paddy fields [J]. J Geochemical Explor, 2014, 147(B): [11],,,. [J]., 2011, 38(11): Kong T, Hao XQ, Zhao ZS, et al. Progress on analysis of heavy metal residues [J]. China Anim Husb Vet Med, 2011, 38(11): [12],,,. [J]., 2012, 18(5): 1 4. Yang F, Meng QX, Peng ZH, et al. Progress in application of inductively coupled plasma mass spectrometry hyphenated technique [J]. Mod Instrum, 2012, 18(5): 1 4. [13],,,. [J]., 2014, 5(8): Wu R, Zhang LX, Li PW, et al. Research progress on analytical methods for heavy metals in grains [J]. J Food Saf Qual, 2014, 5(8): [14] [J]., 2014, 35(18): Qin DL. Simultaneous determination of 28 trace elements in aquatic products by microwave digestion-inductively coupled plasma mass spectrometry method [J]. Sci Technol Food Ind, 2014, 35(18): [15]. (ICP-MS) [J]., 2012, 31(3): Wang Y. Determation of harmful elements Pb, As, Cd, Hg, Cu in Yinzhihuang injection by inductively coupled plasma-mass spectrometry [J]. Chin Wild Plant Resour, 2012, 31(3): [16]. [J]., 2001, 11(4): Liu H. The technical application of the method breaking down the food sample in the special microwave oven for analyzing micro-element [J]. Chin J Health Lab Technol, 2001, 11(4): [17] GB [S]. GB Determination of total arsenic and inorganic arsenic in food [S]. [18] GB [S]. GB Determination of cadmium in food [S]. [19] GB [S]. GB Determination of chromium in food [S]. [20] GB/T [S]. GB/T Tolerance limit of contamination in food [S]. [21] GB [S]. GB National food safety standard--instant noodles [S]. 作者简介 ( 责任编辑 : 姚菲 ) 王绍青, 助教, 主要研究方向为食品质量与安全 @qq.com 朱莉萍, 工程师, 主要研究方向为食品安全 gufeng1979@163.com

Lead and cadmium contents in ceress and pulses in north-eastern China [J]. Sci Total Environ, 1998, 220(2 3): 137 145. [3] Liu XM, Song QJ, Tang Y, et al.

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10