Microsoft Word 张遴-二校

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1 6 2 Vol. 6 No Journal of Food Safety and Quality Feb., 2015 张遴 1*, 钟战强 1, 乔冠华 1, 邓阿粉 2 (1., ; 2., ) 摘要 : 目的方法,, 结果, 0.999, 0.03 μg/kg 0.12 μg/kg, (RSD) 3.5% 8.1%, 96% 116% 结论, 关键词 : ; ; ; ; ; ; Determination of lead, arsenic, cadmium, chromium and mercury by inductively coupled plasma mass spectrometry in frost cosmetics ZHANG Lin 1*, ZHONG Zhan-Qiang 1, QIAO Guan-Hua 1, DENG A-Fen 2 (1. Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi an , China 2. Xi an Yinqiao Paedia Nutrition Co., Ltd., Xi an , China) ABSTRACT: Objective To establish a rapid determination analysis method of lead, cadmium, chromium, arsenic and mercury in frost cosmetics. Methods By microwave digestion for sample pretreatment, lead, cadmium, chromium, arsenic and mercury in frost cosmetics were directly determined by inductively coupled plasma mass spectrometry. The instrument condition was optimized and the methods detection limit, precision and accuracy of methodology were researched. Results With the Cosmetics Health Standard comparison verification method, correlation coefficient > 0.999, the detection limit was between 0.03 μg/kg~0.12 μg/kg, relative standard deviation (RSD) was 3.5%~8.1%, the recovery was 96%~116%. Conclusion Verified by the standard materials with different substrates, the measurements were within the scope of the standard, which showed the method was suitable for rapid determination of lead, cadmium, chromium, arsenic and mercury in the frost cosmetics, and could satisfy the requirements of Cosmetics Health Standard. KEY WORDS: inductively coupled plasma mass spectrometry; cosmetics; lead; cadmium; chromium; arsenic; mercury * 通讯作者 :,, zhanglinder@163.com *Corresponding author: ZHANG Lin, Researcher, Shaanxi Entry-Exit Inspection and Quarantine Bureau, No.10, Hanguang North Road, Shaanxi , China. zhanglinder@163. com

2 引言,,,,,,,,,, [1] ;, [2],, (ICP-MS) [3-13], - (ICP-MS),,,,,,, 2 材料与方法 2.1 仪器与试剂 (ELAN 6100 DRC-e) ( PE ) (MARSXpress)( CEM ) (1000 mg/l)( GB/T 602 ( GSB G )),, 18.5 ΜΩ cm 2.2 标准溶液的配置 : 1000 μg/l,, μg/l : 100 μg/l 2.3 试验方法 0.2 g( g),, 6 ml 2 ml, 12 h, ( : 800 W, 100%, 8 min 120, 2 min; 8 min 160, 5 min; 8 min 190, 20 min),, 25 ml,, 3 结果与分析 3.1 样品前处理的选择,,,,,,,,,, 3.2 仪器工作条件选择,, 24 Mg 5000cps 115 In 25000cps 238 U 20000cps, 156 CeO + / 140 Ce + 3%, 69 Ba 2+ / 138 Ba + 3% Bkgd220 3cps, Bkgd 8.5 3cps,, 1 表 1 仪器参数 Table 1 Instrument parameters 0.93 L/min RF 1250 W 1.2 L/min V 15 L/min 850 V 6.5 V 1.5 s 3.3 同位素和内标的选择及干扰消除 ICP-MS (

3 2, : 701 ) [14-15],,,, 206 Pb 202 Hg 111 Cd 75 As 53 Cr, ±50amu, [9], 197 Au 115 In 72 Ge, 197 Au 115 In 72 Ge,,,,, 10 min, 0.9 ml,,, 0.999,, 0.980,, 3.4 标准曲线的绘制及检出限 , 0.03 μg/kg 0.12 μg/kg, 3.5 准确性试验 (GBW10010) (GBW10016) 5 3, 3 3 :, 3.6 样品检测结果 8,,,, 回收率及精密度试验 6,,, 96% 116%, 2.2% 8.1%, 5 Table 2 表 2 线性回归方程相关系数及检出限 (μg/kg) Linear regression equation, correlation coefficient and detection limit (μg/kg) Pb Y=1.8615X Hg Y=1.8896X Cd Y=0.7259X As Y=0.3331X Cr Y=0.3976X Table 3 表 3 标准物质验证结果 (mg/kg) Standard material verification results (mg/kg) Pb ± ±0.2 Hg ± ± Cd ± ±0.004 As ± ±0.03 Cr (0.09) ±0.10

4 702 6 表 4 样品检测结果 (mg/kg) Table 4 Sample test results (mg/kg) Pb Cd Cr As Hg Table 5 表 5 回收率和精密度试验结果 (mg/kg) Recovery rate and precision test results (mg/kg) RSD% Pb Hg Cd As Cr 结论 8, :,,,,, 5 参考文献 [1] [S] The Cosmetics health standards [S] [2],,,. ICP-OES Pb As Hg[J]., 2008, 27( ): Ni WH, Chen MC, Jian YB, et al. Determination of Pb As Hg using microwave digestion in Cosmetics [J]. Anal Lab, 2008, 27( ): [3] SN/T (ICP-MS) [S]. SN/T Deternation of arsenic, lead, mercury, cadmium in foodstuffs-icp-ms method [S]. [4],,,. ICP-MS [J]., 2010, 10(3): Dai JJ, Liu F, Liang W, et al. The determination of Pb, As, Cd, Hg elements in cosmetics by Inductively coupled plasma-ms spectrometry [J]. Pract Prev Med, 2010, 10(3): [5],,,. ICP-MS [J]., 2010, 27(2), Wang BT, Yan Z, Lin YK, et al. Determination of elements in milk powder by ICP-AES and Disturbance evaluation [J]. Spectrosc Lab, 2010, 27(2): [6],,,. ICP-MS [J]., 2008, 29(3): Liu JH, Jiao H, Wen QL, et al. Determination of Cr, As, Cd, Nd, Pb in cosmetics by ICP-MS [J]. Mass Spectrom Soci, 2008, 29(3): [7],,,. - (ICP-MS) [J]., 2012, 2: Liu SJ, Ping QJ, Yang XJ, et al. Determination of selenium in soybean using microwave digestion-icp-ms [J]. Food Ind, 2012, 2:

2, : 703 [8],,,. - [J]., 2012, 32, 1: 223 228. Wang Y, Guo YL, Yuan HL, et al.

5 2, : 703 [8],,,. - [J]., 2012, 32, 1: Wang Y, Guo YL, Yuan HL, et al. Progress in combination of gel electrophoresis and laser ablation inductively coupled plasma mass spectrometry for trace elements determination in proteins [J]. Spectrosc Spectral Anal, 2012, 32(1): [9],,,. -ICP-ORS-MS 17 [J]., 2011, 30(8): Yu Z, Jiang ZG, Zhang S, et al. Rapid determination of 17 trace elements in cream cosmetics By ORS-ICP-MS with emulsion assistant microwave digestion [J]. Anal Lab, 2011, 30(8): [10]. ICP-MS 5 [J]., 2012, 40(1): Su L. Five kind of metal elements content in rhizoma corydalis by icp-ms method [J]. Guangzhou Chem Ind Technol, 2012, 40(1): [11],,,. ICP-MS [J]., 2012, 33(3): Liu XF, Xue CH, Wang YM, et al. Determination of mineral elements in two kinds of sea urchin by ICP-MS method [J]. Food Sci Technol Ind, 2012, 33(3): [12],,,. - - [J]., 2012, 40(1): Xu JY, Wang T, Chen DJ, et al. Determination of mercury species with inductively coupled plasma-mass spectrometry based on UV-induced chemical vapor generation interface [J]. Anal Chem, 2012, 40(1): [13],,,. ICP-MS [J]., 2012, 29(2): Xue XS, Xu YM, Zhang HR, et al. Determination of hazardous elements in Bruceae Fructus by ICP-MS [J]. Shenyang Pharm Univ, 2012, 29(2): [14],,,. [J]., 2006, 25(6): Liu SQ, Liu CM, Shi YZ, et al. Inductively coupled plasma mass spectrometry determination of eight kinds of harmful metal elements in cosmetics [J]. Environ Chem, 2006, 25(6): [15],,. [J]., 2010, 1: Lin L, Chen G, Chen YH. Determination of metal elements and investigation on arsenic species incream cosmetics [J]. Environ Chem, 2010, 1: 作者简介 ( 责任编辑 : 白洪健 ) 张遴, 研究员, 主要研究方向为食品化妆品等的检验检测 zhanglinder@163.com by high performance liquid Chromatography on-line coupled

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