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1 7 3 Vol. 7 No Journal of Food Safety and Quality Mar., 李梦怡 1, 董喆 1, 费丽娜 2, 曹进 (1., ; 2., ) 1* 摘要 : 目的方法 -, 3 9, 103 Rh 185 Re 结果, ; 9 r ; ; 9 82%~120% ; 7.8% 结论, 3 9 关键词 : ; ; ; Determination of 9 kinds of elements in health food by microwave digestion-inductively coupled plasma mass spectrometry LI Meng-Yi 1, DONG Zhe 1, FEI Li-Na 2, CAO Jin 1* (1. National Institutes for Food and Drug Control, Beijing , China; 2. Jilin Institutes for Food and Drug Control, Jilin , China) ABSTRACT: Objective To establish a method for simultaneous determination of 9 kinds of elements such as Na, Mg, K, Ca, Mn, Fe, Cu, Zn, and Se, in liquid, solid, and soft capsule types of health food by microwave digestion- inductively coupled plasma mass spectrometry (ICP-MS). Methods Nine kinds of elements in 3 kinds of matrix of health food were firstly decomposed by microwave oven with nitric acid and hydrogen peroxide, and then determined simultaneously by ICP-MS. Samples were corrected by adding internal standard solution on line, with 103 Rh and 185 Re as internal standard. Results This method showed a wide linearity range, and low detection limit. The recoveries were in the range of 82%~120%, and relative standard deviations were under 7.8%. Conclusion This method is rapid, sensitive and accurate, and suitable for the simultaneous determination of Na, Mg, K, Ca, Mn, Fe, Cu, Zn, and Se in 3 kinds of matrix of liquid, solid and soft capsule. KEY WORDS: elements; health food; microwave digestion; inductively coupled plasma mass spectrometry * 通讯作者 :,, caojin@nifdc.org.cn *Corresponding author: CAO Jin, Professor, National Institutes for Food and Drug Control, No.2, Tiantanxili, Dongcheng District, Beijing , China. caojin@difdc.org.cn

2 3, : 引言,,,,,,,,,,,,,,, [1,2],,,,,, [3] [4] [5] [6] [7],, [8, 9],,,,,,, [10, 11], 3 9,,,,,,, 2 材料与方法 2.1 仪器与试剂 icap-q, (Thermo Fisher ); MARS5 (CEM ); Milli-Q (Sartorius ); BHW-09C ( ); METTLER AL204 (Mettler Toledo ) (, ); : (Na) (Mg) (K) (Ca) (Mn) (Fe) (Cu) (Zn) [ρ= µg/ml], (Se) [ρ=100.0 µg/ml] ( ); : Re [ρ=10.0 µg/ml] Rh [ρ=10.0 µg/ml]( ); : (Li) (Co) (In) (U) (Ba) (Ce)[ρ=1.0 μg/l] ( ) 2.2 样品前处理 0.3 g,, 5.0 ml, 2.0 ml, min,,,,, 1 表 1 微波消解温度时间程序 Table 1 Time-temperature program for digestion / /min /min ,, ml, 25 ml 2.3 系列标准溶液配制 9, 5%, (Na) 10 mg/l (Mg) 10 mg/l (K) 10 mg/l (Ca) 10 mg/l (Mn) 1 mg/l (Fe) 1 mg/l (Cu) 1 mg/l (Zn) 1 mg/l (Se) 0.5 mg/l

3 ,, 5%,, 表 2 系列标准溶液浓度 (mg/l) Table 2 Concentration of serial standard solutions (mg/l) Na Mg K Ca Mn Fe Cu Zn Se Ⅰ Ⅱ Ⅲ Ⅳ V 样品测定, (Rh Re10 μg/l) : : 1550 W; : 14 L/min; : 1 ml/min; : 0.8 L/min; : 5 mm; : ; : 3 ; : ; : KED; : (>99.999%), : 4.2 ml/min; : 40 r/min; : 0.02 s 3 结果与分析 3.1 消解方法及条件的选择, [13],,, ; ICP-MS, 3, 2, -, 9,,, 测定同位素的选择 40 Ca, 40 Ar 40,, 44 Ca 56 Fe, ( 40 Ar+ 16 O) 56, 57 Fe, 3.3 线性范围,, (Rh Re10 μg/l), ICP-MS X, Y,, ,,, 0.999, 3.4 检出限与定量限 , (SD), 3, ; 10, [14] 0.3 g, 25 ml,, 加标回收率, 3, 6, 2.2,,, 5, 3 82%~120%, 93%~117%, 93%~119%, 3.6 精密度 ,, RSD 2.2 3, 3, 1,, RSD 6

4 3, : Table 3 表 3 各元素线性方程相关系数及线性范围 Linear equations, correlation coefficients and linear range for each element r (mg/kg) 23 Na Y= X ~10 24 Mg Y= X ~10 39 K Y=814098X ~10 44 Ca Y=55379X ~10 55 Mn Y=15230X ~1 57 Fe Y=621X ~1 63 Cu Y=32737X ~1 66 Zn Y=4971X ~1 78 Se Y=429X ~0.5 Table 4 表 4 检出限与定量限 (mg/kg) LOD and LOQ of the method (mg/kg) 23 Na Mg K Ca Mn Fe Cu Zn Se Table 5 表 5 加标回收率 (n=6) Recovery test of the method (n=6) 23 Na 120% 119% 120% 106% 112% 106% 111% 117% 105% 24 Mg 106% 110% 111% 104% 104% 105% 109% 108% 106% 39 K 104% 107% 93% 101% 106% 106% 106% 110% 106% 44 Ca 82% 114% 126% 97% 105% 115% 103% 111% 116% 55 Mn 101% 104% 99% 106% 106% 107% 110% 110% 107% 57 Fe 88% 115% 109% 99% 105% 102% 106% 109% 103% 63 Cu 104% 103% 99% 101% 97% 98% 104% 100% 100% 66 Zn 93% 98% 97% 117% 93% 104% 119% 94% 107% 78 Se 87% 94% 104% 93% 94% 106% 93% 95% 111%

5 948 7 表 6 精密度试验结果 Table 6 Results of precision test (n=6) (n=3) 23 Na 2.4% 2.7% 2.6% 5.3% 0.9% 4.0% 24 Mg 2.4% 2.4% 2.6% 2.0% 0.7% 2.4% 39 K 1.8% 2.0% 2.6% 4.5% 2.8% 5.0% 44 Ca 2.5% 2.7% 7.8% 6.3% 2.3% 5.0% 55 Mn 2.0% 2.5% 3.2% 2.1% 1.1% 2.4% 57 Fe 2.1% 2.5% 3.1% 2.8% 0.4% 1.8% 63 Cu 2.3% 2.5% 2.8% 2.0% 1.9% 3.0% 66 Zn 4.6% 3.1% 4.4% 1.5% 2.3% 0.4% 78 Se 4.1% 2.1% 3.0% 3.4% 2.8% 4.3% 3.7 稳定性, 3, h, RSD, 7, 24 h 表 7 样品稳定性 (n=4) Table 7 Results of stability test (n=4) 23 Na 3.0% 3.3% 4.6% 24 Mg 3.5% 3.8% 4.7% 39 K 4.6% 5.0% 6.2% 44 Ca 4.7% 4.6% 6.2% 55 Mn 3.0% 3.0% 4.8% 57 Fe 2.6% 2.5% 4.4% 63 Cu 2.8% 1.8% 2.8% 66 Zn 6.6% 2.8% 2.7% 78 Se 5.0% 5.0% 5.3% 3.8 样品测定 8, 8 4 讨论 4.1 基质干扰,,,,, -,, 9,,,,,,,,, 检测干扰的消除 ICP-MS,

6 3, : 表 8 Table 8 样品含量测定结果 (mg/kg) Results of sample test (mg/kg) ND 120 ND 2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND : ND 3 [15], ;, [16],, / 5 结论,,,, 3 9 参考文献 [1],,. [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. [2]. [J]., 2014, 30(2): Jiang N. Application and research progress of inductively coupled plasma mass spectrometry in environmental monitoring area [J]. Environ Monitor China, 2014, 30(2): [3]. - [J]., 2014, (11): Zhang JY. Simultaneous determination of trace elements and major elements in food by ICP-MS using microwave digestion for sample preparation [J]. Chin J Anal Chem, 2014, (11): [4],,,. - [J]., 2013, 29(4): Ni ZL, Tang FB, Qu MH, et al. Determination of arsenic species in scented tea by HPLC-ICP-MS [J]. J Anal Sci, 2013, 29(4): [5],,. - [J]., 2013, 34(12): Yan N, Zhao SG, Gao YY. Determination of cadmium, mercury, lead and chromium in alcoholic drinks by inductively coupled plasma-mass spectrometry with dynamic reaction cell [J]. Food Sci, 2013, 34(12): [6] [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): [7],. [J]., 2014, (7): Jiang HL, Xu XQ. Simultaneous determination of heavy metals in honeysuckle by ICP-MS[J]. J Anhui Agric Sci, 2014,

950 7 (7):1927 1928. [8],,,. - 25 [J]., 2014, 45(15): 2172 2177. Tang WG, Wang QZ, Yin M, et al.

- [J]., 2014, (04): 462 465. Liu W, Hu JD, Yang HX, et al.

7 950 7 (7): [8],,, [J]., 2014, 45(15): Tang WG, Wang QZ, Yin M, et al. Determination of 25 kinds of minerals in mailuoning injection by inductively coupled plasma mass pectrometry with microwave digestion [J]. Chin Tradit Herbal Drug, 2014, 45(15): [9],,,. - [J]., 2014, (04): Liu W, Hu JD, Yang HX, et al. Rapid determination of inorganic arsenic in natural water by high performance liquid chromatography inductively coupled plasma mass spectrometry[j]. Chin J Anal Lab, 2014, (04): [10],,,. - 6 [J]., 2013, 41(11): Wang X, Xing YN, Chen ZY, et al. Determination of inorganic selenium in selenium-enriched foods by high performance liquid chromatography inductively coupled plasma mass spectrometry [J]. Chin J Anal Chem, 2013, 41(11): [11] NY/T [S]. NY/T Determination for mineral elements in vegetables, fruits and derived products -Inductively coupled plasma atomic emission spectrometry [S]. [12] GB [S]. GB National standards for food safety-determination of rare earths in vegetable foods [S]. [13],,,. [J]., 2014, 28(11): Feng KR, Liu HJ, Wei Y, et al. Proficiency testing on the determination of chromium in cosmetic emulsion [J]. Chin Pharm Affairs, 2014, 28(11): [14] GB/T [S]. GB/T Detection limit and quantitative limit of analysis method [S]. [15],,,. 15 [J]., 2009, 38(6): Tian PY, Liu YH, Wang P, et al. Fifteen rare earth elements in cosmetics determinated by inductively coupled plasma-mass spectrometry [J]. J Hyg Res, 2009, 38(6): [16] 喆,,,. 37 [J]., 2015, 38(6): Dong Z, Li MY, Pan WJ, et al. Determination of 37 elements in cosmetics by inductively coupled plasma-mass spectrometry [J]. Deter Cosm, 2015, 38(6): 作者简介 ( 责任编辑 : 杨翠娜 ) 李梦怡, 硕士, 助理研究员, 主要研究方向为食品安全检测 limengyi@nifdc.org.cn 曹进, 博士, 研究员, 主要研究方向为食品安全检测 caojin@nifdc.org.cn

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.