超级微波消解-ICP-MS法测定洗发类化妆品中37种元素

doi:10.3969/j.issn.2097-2806.2023.05.016

摘要/Abstract

摘要：

采用超级微波消解-电感耦合等离子体质谱（ICP-MS）建立了洗发类化妆品中37种元素含量的测定分析方法。样品经超级微波消解仪消解后，采用铼（Re）、铑（Rh）作为内标元素，采用ICP-MS同时测定洗发类化妆品中铅（Pb）、砷（As）、汞（Hg）、镉（Cd）、锂（Li）、铍（Be）、钪（Sc）、钒（V）、钴（Co）、镍（Ni）、铬（Cr）、锰（Mn）、铜（Cu）、铷（Rb）、锶（Sr）、镨（Pr）、钕（Nd）、镝（Dy）、银（Ag）、铟（In）、铯（Cs）、钡（Ba）、铊（Tl）、铋（Bi）、钍（Th）、镧（La）、铈（Ce）、铒（Er）、铕（Eu）、钆（Gd）、钬（Ho）、镥（Lu）、钐（Sm）、铽（Tb）、铥（Tm）、钇（Y）、镱（Yb）37种元素的含量。该方法在一定浓度范围内线性关系良好，线性相关系数均≥0.995 0，低、中、高浓度加标回收率范围为87.1%~113.5%，RSD为0.72%~5.00%（n=6）。该方法专属性强、灵敏度高、可快速、准确测定洗发用品中37种金属元素。

关键词: 超级微波消解, 电感耦合等离子体质谱法, 洗发类化妆品, 元素

Abstract:

A method for determination of 37 elements in shampoo cosmetics was established by using super microwave digestion-inductively coupled plasma mass spectrometry （ICP-MS）. After the samples were digested on a super microwave digester, Re and Rh were applied as internal standard elements, and the concentrations of 37 elements including Pb, As, Hg, Cd, Li, Be, Sc, V, Co, Ni, Cr, Mn, Cu, Rb, Sr, Pr, Nd, Dy, Ag, In, Cs, Ba, Tl, Bi, Th, La, Ce, Er, Eu, Gd, Ho, Lu, Sm, Tb, Tm, Y and Yb were simultaneously determined by ICP-MS. The method has a good linear relationship within a certain concentration range, and the linear correlation coefficients are all≥0.995. The recovery rates of low, medium and high spiked concentrations are 87.1%-113.5%, and the RSD is 0.72%-5.00% （n=6）. This method has strong specificity and high sensitivity, which can rapidly and accurately determine 37 metal elements in shampoo products.

Key words: super microwave digestion, ICP-MS, shampoo cosmetics, element

中图分类号:

TQ658

尹伟成, 王彦超, 徐少康, 吴志珊, 唐桂鹏, 张伟清. 超级微波消解-ICP-MS法测定洗发类化妆品中37种元素[J]. 日用化学工业（中英文）, 2023, 53(5): 602-608.

Yin Weicheng, Wang Yanchao, Xu Shaokang, Wu Zhishan, Tang Guipeng, Zhang Weiqing. Determination of 37 elements in shampoo cosmetics by super microwave digestion-inductively coupled plasma mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2023, 53(5): 602-608.

图/表 3

表 1

37种元素的线性范围和检出限"

元素	线性方程	线性范围/（μg/L）	相关系数r	检出限/（μg/L）	检出浓度/（μg/kg）
⁷Li	y=2.113 0×10^-5x+6.110 2×10^-7	0~100	0.998 6	0.060 0	5.00
⁹Be	y=3.044 4×10^-5x+2.835 4×10^-7	0~100	0.998 6	0.020 0	2.00
⁴⁵Sc	y=0.001 4x+4.247 0×10^-5	0~100	0.999 1	0.006 0	0.40
⁵¹V	y=0.003 5x+3.075 8×10^-5	0~100	0.996 8	0.007 0	0.60
⁵²Cr	y=0.004 9x+2.418 2×10^-4	0~100	0.997 2	0.010 0	0.90
⁵⁵Mn	y=0.003 1x+1.970 2×10^-4	0~100	0.998 3	0.030 0	2.00
⁵⁹Co	y=0.008 1x+3.160 5×10^-5	0~100	0.997 7	0.006 0	0.50
⁶⁰Ni	y=0.002 7x+1.789 5×10^-5	0~100	0.999 0	0.200 0	18.00
⁶³Cu	y=0.005 9x+0.183 4×10^-4	0~100	0.999 2	0.060 0	5.00
⁷⁵As	y=7.252 4×10^-4x+1.853 7×10^-5	0~100	0.998 9	0.010 0	0.90
⁸⁵Rb	y=0.003 1x+3.156 0×10^-5	0~100	0.999 1	0.009 0	0.80
⁸⁸Sr	y=0.004 0x+7.926 8×10^-4	0~100	0.997 0	0.050 0	4.00
⁸⁹Y	y=0.008 4x+3.208 4×10^-5	0~100	0.997 8	0.006 0	0.50
¹⁰⁷Ag	y=0.012 0x+7.681 4×10^-5	0~100	0.997 5	0.001 0	0.08
¹¹¹Cd	y=0.002 4x+3.569 7×10^-6	0~100	0.999 2	0.004 0	0.40
¹¹⁵In	y=0.011 8x+4.814 9×10^-5	0~100	0.997 7	0.007 0	0.60
¹³³Cs	y=0.009 8x+2.992 8×10^-5	0~100	0.997 7	0.004 0	0.30
¹³⁷Ba	y=0.002 1x+1.560 1×10^-4	0~100	0.999 2	0.200 0	13.00
¹³⁹La	y=0.023 6x+1.990 5×10^-4	0~100	0.998 9	0.005 0	0.40
¹⁴⁰Ce	y=0.028 6x+3.399 4×10^-4	0~100	0.998 9	0.007 0	0.60
¹⁴¹Pr	y=0.030 7x+1.003 0×10^-4	0~100	0.998 9	0.004 0	0.30
¹⁴⁶Nd	y=0.008 6x+5.366 4×10^-5	0~100	0.998 3	0.003 0	0.20
¹⁴⁷Sm	y=0.007 4x+2.738 0×10^-5	0~100	0.998 1	0.003 0	0.20
¹⁵³Eu	y=0.026 1x+6.094 2×10^-5	0~100	0.999 2	0.004 0	0.30
¹⁵⁷Gd	y=0.010 9x+4.407 2×10^-5	0~100	0.998 0	0.004 0	0.40
¹⁵⁹Tb	y=0.069 0x+1.309 7×10^-4	0~100	0.999 7	0.004 0	0.30
¹¹⁶³Dy	y=0.016 2x+3.671 5×10^-5	0~100	0.998 9	0.004 0	0.40
¹⁶⁵Ho	y=0.070 2x+1.214 7×10^-4	0~100	0.999 8	0.004 0	0.30
¹⁶⁶Er	y=0.021 0x+4.124 1×10^-5	0~100	0.999 3	0.004 0	0.40
¹⁶⁹Tm	y=0.077 8x+1.323 0×10^-4	0~100	0.999 8	0.003 0	0.30
¹⁷²Yb	y=0.017 2x+3.848 1×10^-5	0~100	0.999 0	0.003 0	0.30
¹⁷⁵Lu	y=0.052 4x+9.247 6×10^-5	0~100	0.999 6	0.003 0	0.30
²⁰²Hg	y=1.706 6×10^-4x+7.848 6×10^-5	0~4	0.998 4	0.009 0	0.80
²⁰⁵Tl	y=0.053 1x+7.644 1×10^-4	0~100	0.999 7	0.004 0	0.40
²⁰⁸Pb	y=0.036 7x+0.001 9	0~100	0.999 6	0.010 0	1.00
²⁰⁹Bi	y=0.057 8x+0.001 3	0~100	0.999 7	0.003 0	0.20
²³²Th	y=0.075 0x+0.001 9	0~100	0.999 9	0.000 9	0.08

表 1

表 2

表 3

参考文献 16

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元素名称	低质量浓度加标		中质量浓度加标		高质量浓度加标
元素名称	平均回收率	RSD/%	平均回收率	RSD/%	平均回收率	RSD/%
⁷Li	95.2	3.80	100.0	3.72	99.3	3.12
⁹Be	93.9	4.51	103.5	3.01	99.5	3.24
⁴⁵Sc	93.0	1.33	100.0	4.34	101.6	0.96
⁵¹V	102.0	4.79	102.9	2.13	108.5	3.84
⁵²Cr	104.0	1.95	104.6	1.72	107.3	2.11
⁵⁵Mn	97.2	3.37	101.2	1.53	98.5	1.75
⁵⁹Co	100.4	4.07	99.8	2.65	100.5	3.70
⁶⁰Ni	94.2	3.67	100.7	2.85	97.2	2.75
⁶³Cu	102.9	4.71	107.3	2.06	110.3	2.18
⁷⁵As	95.0	3.16	99.6	2.88	97.0	5.00
⁸⁵Rb	95.0	1.43	101.0	1.47	98.0	0.72
⁸⁸Sr	96.5	3.40	99.2	2.67	107.9	3.71
⁸⁹Y	103.4	3.23	100.5	1.84	103.9	2.58
¹⁰⁷Ag	103.2	4.18	99.9	2.38	103.9	2.55
¹¹¹Cd	98.0	4.33	99.3	3.26	97.9	2.49
¹¹⁵In	100.2	3.09	100.6	2.84	102.6	3.32
¹³³Cs	100.2	4.00	100.6	2.27	102.8	2.94
¹³⁷Ba	97.3	4.52	101.2	3.04	99.3	1.80
¹³⁹La	105.4	3.60	98.2	3.25	111.4	2.31
¹⁴⁰Ce	102.4	3.69	98.5	2.00	104.5	2.83
¹⁴¹Pr	102.4	4.21	98.2	1.82	103.1	2.31
¹⁴⁶Nd	103.5	3.97	111.5	2.04	108.1	0.87
¹⁴⁷Sm	102.9	2.73	100.3	2.02	106.6	2.86
¹⁵³Eu	106.5	3.12	101.5	1.84	106.8	3.06
¹⁵⁷Gd	106.1	3.22	101.9	1.90	101.3	2.69
¹⁵⁹Tb	102.2	2.43	99.7	1.88	110.5	1.83
¹¹⁶³Dy	99.6	2.66	100.0	1.63	99.6	1.15
¹⁶⁵Ho	100.4	4.08	99.3	2.18	99.2	2.31
¹⁶⁶Er	99.9	3.33	99.4	2.11	100.8	3.54
¹⁶⁹Tm	99.6	3.40	99.1	2.10	102.0	2.92
¹⁷²Yb	99.0	3.30	98.0	1.28	100.8	2.88
¹⁷⁵Lu	99.7	3.39	99.0	2.13	100.3	2.76
²⁰²Hg	106.1	4.68	99.0	3.37	100.4	2.78
²⁰⁵Tl	99.7	2.84	98.3	1.69	104.0	3.18
²⁰⁸Pb	98.6	3.70	101.2	2.08	101.2	3.54
²⁰⁹Bi	100.1	2.62	99.3	1.49	101.2	2.44
²³²Th	101.7	3.32	99.5	2.00	100.6	2.87

元素	检出浓度/（mg/kg）
元素	样品1	样品2	样品3	样品4	样品5	样品6	样品7	样品8	样品9
⁷Li	0.056	0.048	—	—	—	0.018	0.043	0.019	—
⁴⁵Sc	—	ND	0.016	ND	ND	0.010	—	0.062	ND
⁵¹V	—	—	—	ND	—	—	—	0.730	ND
⁵²Cr	0.10	0.050	0.073	0.057	0.068	0.160	0.360	0.250	0.140
⁵⁵Mn	—	—	ND	ND	ND	0.32	—	0.97	—
⁶⁰Ni	0.061	0.039	0.043	0.061	0.062	0.100	0.170	0.700	0.088
⁶³Cu	ND	ND	ND	ND	ND	—	—	8.10	ND
⁷⁵As	0.011	0.006 2	0.020	0.004 0	0.008 1	0.004 3	0.004 6	0.047	—
⁸⁵Rb	0.015	—	0.049	—	—	0.834	4.529	—	—
⁸⁸Sr	0.310	0.120	0.094	0.091	0.084	0.140	0.130	0.290	0.160
⁸⁹Y	ND	ND	ND	ND	ND	ND	ND	0.229	ND
¹⁰⁷Ag	0.003 4	—	0.006 0	—	—	—	—	—	ND
¹¹¹Cd	ND	ND	ND	ND	ND	ND	ND	0.012	ND
¹³³Cs	—	ND	ND	ND	ND	0.006 5	0.011	0.001 5	ND
¹³⁷Ba	—	—	—	0.13	—	0.12	0.12	0.12	—
¹⁴⁰Ce	0.015 0	0.005 9	0.006 3	0.005 4	0.006 7	0.006 0	0.005 9	0.270 0	0.005 2
¹⁴⁶Nd	0.006 6	—	—	—	0.008 5	—	—	0.005 9	—