Microsoft Word 姜新二校出1808

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1 7 5 Vol. 7 No Journal of Food Safety and Quality May, 姜新 *, 刘德晔, 刘华良 (, ) 摘要 : 目的 - - 方法 - (4:1, V:V) 230, - ; 结果 4.0%, 2.0% 2.0~40.0 ng/ml, , ng/ml, 93.0%~102.0%, 2.2%(n=6) 结论, 关键词 : ; ; - Determination of total selenium in selenium nutrition enhancer by refluxing wet digestion-hydride generation-atomic fluorescence spectrometry JIANG Xin *, LIU De-Ye, LIU Hua-Liang (Jiangsu Provincial Center for Disease Control and Prevention, NanJing , China) ABSTRACT: Objective To establish a method for the determination of total selenium in nutrition enhancer by hydride generation-atomic fluorescence spectrometry (HG-AFS) with refluxing wet digestion Methods The nitric acid-perchloric acid (4:1, V:V) was used as the digestion system with reflux digestion temperature of 230. Samples were detected by the method of hydride generation-atomic fluorescence spectrometry. And then the effects of digestion system, reducing agent and masking agent on fluorescence intensity were investigated. Results The fluorescence intensity was the strongest using 4.0% hydrochloric acid as acid medium and 2.0% potassium borohydride. Selenium had a good linear relationship in the range of 2.0~40.0 ng/ml with the correlation coefficient of The limit of detection was ng/ml. The recovery rates at 3 spiked levels were in the range of 93.0%~102.0%, and RSD was 2.2% (n=6) Conclusion This method is simple, rapid, and accurate, and reliable for the determination of total selenium in selenium nutrition enhancer KEY WORDS: selenium nutrition enhancer; total selenium; hydride generation-atomic fluorescence spectrometry (HG-AFS) * 通讯作者 :,,, @qq.com *Corresponding author: JIANG Xin, Associate Chief Technician, Jiangsu Provincial Center for Disease Control and Prevention, No.172, Jiangsu Road, Nanjing , China @qq.com

2%(n=6) 结论, 关键词 : ; ; - Determination of total selenium in selenium nutrition enhancer by refluxing wet digestion-hydride generation-atomic fluorescence spectrometry JIANG Xin *, LIU De-Ye, LIU

2 5, : 引言, [1,2],, (FAO/WHO/IAEA) 40 μg/d 30 μg/d [3], [4,5],, [6,7], - [8-10] [11-13] GB [14],, - -, 2 材料与方法 2.1 仪器与试剂 AFS830a ( ); EH35B ( ); ML503 ( ) (, ) (, ) (, ); (, ) (, ) (, ) 20% 24 h, 1000 μg/ml ( : GSB , ), u=0.7%(k=2), : 14A 实验方法溶液的配制 2.0% (m:v)+ 0.5% (m:v) : 2.0 g 0.5%, ; 1000 μg/ml: 1.0 μg/ml, 1.0% 样品前处理 10,, g 150 ml, 3~4, - 10 ml,, 230 ( ),, 25 ml, 1.0 ml, 25 ml,, 4.0% 仪器条件 80 ma 40 ma, 270 V, 300 ml/min, 800 ml/min, 8 mm,, : 0.5 ml, 样品测定,,, 3 结果与讨论 3.1 实验条件的优化消解体系及消解温度的选择 [15,16],,,, 230,,,, 消解体系中盐酸溶液的作用 GB [14] -, 6 mol/l, 6 4, 4,, -,,,,, 硼氢化钾浓度的选择 20.0 ng/ml, 4.0%,, 2.0%,, 1 1.0%, 1 s ; 2.0%,, ;,, 3.0%,,

5% (m:v) : 2.0 g 0.5%, ; 1000 μg/ml: 1.0 μg/ml, 1.0% 2.2.2 样品前处理 10,, 0.500 g 150 ml, 3~4, - 10 ml,, 230 ( ),, 25 ml, 1.0 ml, 25 ml,, 4.0% 2.2.3 仪器条件 80 ma 40 ma, 270 V, 300 ml/min, 800 ml/min, 8 mm,, : 0.

3 1810 7, ; 4.0%,, 1 Fig. 1 Effects of concentration of KBH 4 solution on fluorescence intensity of selenium 2,, 酸介质种类及浓度的选择,, ;,, ;,, 20.0 ng/ml, 2.0% ( 0.5% ),, 2.0% 3.0%,, 4.0%,,,, 3 4.0% 共存离子的干扰及消除, [17-20] 40 ng/ml,, ; Hg 2+ As 3+ Pb ng/ml,,,, 2 Fig. 2 Comparison of the morphology of the integral spectrums under different concentrations of KBH 4

0 ng/ml, 2.0% ( 0.5% ),, 2.0% 3.0%,, 4.0%,,,, 3 4.0% 3.1.

4 5, : %~102.0%, 表 1 方法精密度 (n=6) Table 1 RSD of the method (n=6) /(mg/kg) RSD/% Fig. 3 3 Effects of concentration of HCl solution (V/V) on fluorescence intensity of selenium 表 2 3 个水平的加标回收率 Table 2 Recovery rates at 3 spiked levels 3.2 标准曲线和检出限 25 ml, 10 ml, 1.0 ml, 25.0 ml, ng/ml,,, Y=87.93X 6.30, r= , DL=3Sd/k(Sd, k ) ng/ml 3.3 方法的精密度和回收率 6, 1, RSD 2.2%,, RSD 5.0%, 3, 3,, 2, 3 /(mg/kg) /(mg/kg)(n=3) /% 样品分析结果,, 3 4 结论 - - -, 230,, Table 3 表 3 营养强化剂中总硒的测定结果 Analytical results of total selenium in nutrition supplements (mg/kg) C D ( ) E ( ) E 48.8

30, r=0.9999 11, DL=3Sd/k(Sd, k ) 0.028 ng/ml 3.3 方法的精密度和回收率 6, 1, RSD 2.2%,, RSD 5.0%, 3, 3,, 2, 3 /(mg/kg) /(mg/kg)(n=3) /% 0.0 13.5-5.0 18.6 102.0 10.0 22.8 93.0 20.0 32

5 1812 7,, -,,,,, 参考文献 [1],,. [J]., 2010, 120(4): Lu L, Lu B, WANG CE. Analysis of organic selenium and inorganic selenium in health foods [J]. Chin J Health Lab Technol, 2010, 120(4): [2],. 4 N- -N'- -N- [J]., 2008, 37(4): Yang WJ, Chen J, Li WD, et al. Preventive effects of 4 Se-enriched plants on rat stomach cancer induced by MNNG 3. Se accumulation and distribution in rats of different selenium resources for prevention of stomach cancer [J]. J Hyg Res, 2008, 37(4): [3],,,. - - (HPLC-HG-AFS) [J]., 2013, 4(6): Shang DR, Qin DY, Zhao YF, et al. Selenium speciation analysis in aquatic products by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry [J]. J Food Saf Qual, 2013, 4(6): [4] Dumont E, Vanhaecke F, Cornelis R. Selenium speciation from food source to metabolites: a critical review [J]. Anal Bioanal Chem, 2006, 386: [5] Zhang ZY, You Y, Guo QQ, et al. Preliminary study on the standard of selenium content in agricultural products [J]. Asian Agr Res, 2012, 4(10): [6] FOSTER LH, SUMAR S. A rapid microwave-based digestion method for the determination of selenium in infant formulae by means of hydride generation atomic absorption spectrometry (HGAAS) [J]. Food Res, 1996, 40(3): [7],. [J]., 2002, 21(4): Feng SC, Han CX. Determination of trace selenium in serum using matrix modifier by GF-AAS [J]. Chin J Anal Lab, 2002, 21(4): [8],,,. - [J]., 2014, 35(20): Lu L, Liu EL, Chen WR, et al. Determination of Selenium in infant formula by microwave digestion-hydride generation atomic fluorescence spectrometry [J]. Food Sci, 2014, 35(20): [9],,,. - [J]., 2013, 33(24): Wu QH, Huang BX, Ran WQ, et al. Determination of selenium in edible mushrooms by ultrasonic assisted water bath digestion-atomic fluorescence spectrometry [J]. Food Sci, 2013, 33(24): [10],. [J]. Chen YH, Shen RF. Determination of selenium in tea by wet resolution atom fluorescence method [J]. Chin J Health Lab Technol, 2010, 20(10): [11],,,. HPLC_ICP_MS [J]., 2015, 25(5): Xie Q, Li JH, Huang WY, et al. Determination of seleno amino acids in selenium protein by HPLC ICP-MS [J]. Chin J Health Lab Technol, 2015, 25(5): [12],,,. HPLC-DRC-ICP-MS [J]., 2013, 32(2): Ni ZL, Tang FB, Zhang W, et al. Determination of selenium species in Se-enriched vegetables by HPLC-DRC-ICP-MS [J]. Chin J Anal Lab, 2013, 32(2): [13],, 鋆,. HPLC-ICP-MS [J]., 2014, 36(5): Wu YY, Gui RY, Tang J, et al. Analysis of six selenium species in bamboo shoot by HPLC-ICP-MS [J]. Acta Nutr Sin, 2014, 36(5): [14] GB [S]. GB National standards for food safety- Determination of selenium in foods [S]. [15],,,. [J]., 2014, 24(10): Gu YQ, Feng RW, Li ZQ, et al. Improvement of hydride generationatomic fluorescence spectrometry method for determination of selenium in food [J]. Chin J Health Lab Technol, 2014, 24(10): [16],. [J]., 2013, 38(6): 1 5. Yang YL, Liu YY. Determination and speciation analysis progress of selenium in food [J]. China Cond, 2013, 38(6): 1 5. [17] Zhu YG, Pilon-Smits EA, Zhao FJ, et al. Selenium in higher plants: understanding mechanisms for biofortification and phytoremediation [J]. Trends Plant Sci, 2009, 14(8): [18],,, - [J]., 2012, 32(5): Gou TZ, Tang WH, Zhang WH, et al. Determination of selenium in plant samples by hydride generation atomic fluorescence spectrometry [J]. Spectrosc Spect Anal, 2012, 32(5): [19],,,. HG-AFS [J]., 2015, 41(3): Xu LP, Zhao XY, Yang H, et al. The influence of different digestion methods for the determination of selenium in plant samples by HG-AFS [J]. China Meas Test, 2015, 41(3): [20] Montes-Bayon M. Initial studies of selenium speciation in Brassica juncea by LC with ICP-MS and ES-MS detection: an approach for phytoremediation studies [J]. Anal Chem, 2002, 74(1): 作者简介 ( 责任编辑 : 姚菲 ) 姜新, 硕士, 副主任技师, 主要研究方向为食品理化检验 @qq.com, 2010, 20(10):

Preventive effects of 4 Se-enriched plants on rat stomach cancer induced by MNNG 3. Se accumulation and distribution in rats of different selenium resources for prevention of stomach cancer [J].

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

Microsoft Word 姜新 二校出1808

Microsoft Word 姜新二校出1808