微波消解-原子荧光光谱法同时测定化妆品中砷、锑、铅和汞

doi:10.3969/j.issn.1001-1803.2019.11.012

摘要/Abstract

摘要：

建立了微波消解-原子荧光光谱法同时检测化妆品中砷、锑、铅和汞4种有害元素含量的方法。经微波消解仪消解的样品溶液,在预处理加热仪上120 ℃赶酸后,用氢化物发生双道原子荧光光谱仪以1.0%硝酸为载流,5.0%硫脲-抗坏血酸为还原剂同时测定砷、锑、铅和汞。结果表明,砷、锑、铅和汞4种元素在相应的浓度范围内线性良好,相关系数R ²分别为0.999 3,0.998 4,0.997 3和0.999 7。4种元素的加标回收率为91.7%~101.9%。此方法具有操作简便、快速、线性范围宽、适用性强等优点。

关键词: 微波消解, 原子荧光光谱法, 化妆品

Abstract:

A method for the simultaneous determination of arsenic, antimony, lead and mercury in cosmetics by microwave digestion atomic fluorescence spectrometry was established. After the sample solution was decomposed by microwave digester, acid was removed at 120 ℃ on the pretreatment heater. And then arsenic, antimony, lead and mercury were simultaneous determined by hydride generation dual channel atomic fluorescence spectrometer with 1.0% nitric acid as carrier and 5.0% thiourea-ascorbic acid as reductant. The results show that the linearity of arsenic, antimony, lead and mercury is good in the corresponding concentration range, and the correlation coefficients R ² are 0.999 3, 0.998 4, 0.997 3 and 0.999 7, respectively. The recovery of four elements is 91.7%-101.9%. This method has the advantages of simple operation, fast speed, wide linear range and strong applicability.

Key words: microwave digestion, atomic fluorescence spectrometry, cosmetics

中图分类号:

TQ658

周霞,王延华,姜新杰,常澍,孙芬芳. 微波消解-原子荧光光谱法同时测定化妆品中砷、锑、铅和汞[J]. 日用化学工业, 2019, 49(11): 764-768.

ZHOU Xia,WANG Yan-hua,JIANG Xin-jie,CHANG Shu,SUN Fen-fang. Simultaneous determination of arsenic, antimony, lead and mercury in cosmetics by microwave digestion-atomic fluorescence spectrometry[J]. China Surfactant Detergent & Cosmetics, 2019, 49(11): 764-768.

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参考文献 16

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阶段	压力/MPa	温度/℃	时间/min	功率/W
1	2	100	2	400
2	7	130	2	500
3	10	150	30	600

元素	As	Sb	Hg	Pb
灯电流/mA	30	30	24	30
负高压/V	280	280	280	280
原子化器高度/mm	8	8	8	8
载气流量/（mL·min^-1）	300	300	300	300
屏蔽气流量/（mL·min^-1）	600	600	600	600
读数时间/s	12	12	13	13
石英炉温度/℃	180	180	180	180

	线性方程	线性范围/（μg·L^-1）	相关系数	检出限/（μg·L^-1）	相对标准偏差/%
As	y=57.808x+11.357	0~100	0.999 3	0.125 4	0.640
Sb	y=43.375x-23.66	0~100	0.998 4	0.117 6	0.451
Pb	y =946.53x+29.188	0~500	0.997 3	0.424 9	1.820
Hg	y =1 099.2x-13.501	0~ 10	0.999 7	0.011 7	1.210

元素	本底值/（mg·kg^-1）	加标量/（mg·kg^-1）	测定值/（mg·kg^-1）	回收率/%
As	0.125 4	0.250 0	0.375 0	99.8
	0.178 4	5.000 0	5.007 1	96.7
	0.187 6	15.000 0	15.195 2	100.05
Sb	0.185 7	0.250 0	0.423 5	95.1
	0.204 2	5.000 0	5.303 1	101.9
	0.205 8	15.000 0	15.038 5	98.9
Pb	0.085 3	0.250 0	0.319 1	93.5
	0.088 5	25.000 0	23.181 8	92.4
	0.168 1	45.000 0	41.419 2	91.7
Hg	0.046 7	0.250 0	0.278 3	92.6
	0.036 2	0.500 0	0.510 1	94.7
	0.019 0	0.750 0	0.736 7	95.8

样品		测定值/（mg·kg^-1）
样品		As	Sb	Hg	Pb
美白类	A	0.182 6	0.169 4	0.023 4	0.127 6
	B	0.194 3	0.236 6	0.138 1	0.212 4
	C	0.200 1	0.169 2	0.157 0	0.314 3
防晒类	A	0.182 2	0.171 2	0.486 1	0.242 7
	B	0.171 1	0.172 3	0.610 9	0.120 6
	C	0.199 8	0.185 4	0.066 6	0.355 9
保湿类	A	0.201 4	0.171 3	0.011 1	0.089 6
	B	0.184 8	0.174 2	0.027 9	0.039 2
	C	0.176 5	0.266 2	0.117 2	0.076 4
祛斑类	A	0.187 6	0.205 2	0.019 0	0.168 1
	B	0.125 4	0.185 7	0.046 7	0.085 3
	C	0.182 9	0.303 4	0.081 9	0.119 4