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福建省食品药品质量检验研究院,福建 福州 350012
郑景峰,硕士,主任药师,研究方向:药品、化妆品、医疗器械检验和研究,E-mail 625875097@qq.com
陈在敏,硕士,主任药师,研究方向:中药质量控制研究,E-mail:yyhczm@sina.com
收稿日期:2024-10-15,
修回日期:2024-11-30,
录用日期:2024-12-13,
纸质出版日期:2025-05-15
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卢端萍,程佳华,洪清玲,陈旭,陈硕,简育莹,郑景峰,陈在敏.顶空-气相色谱-质谱法测定防晒类化妆品中16种苯系物[J].分析测试学报,2025,44(05):860-867.
LU Duan-ping,CHENG Jia-hua,HONG Qing-ling,CHEN Xu,CHEN Shuo,JIAN Yu-ying,ZHENG Jing-feng,CHEN Zai-min.Determination of 16 Benzene Series in Sunscreen Cosmetics by Headspace-Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(05):860-867.
卢端萍,程佳华,洪清玲,陈旭,陈硕,简育莹,郑景峰,陈在敏.顶空-气相色谱-质谱法测定防晒类化妆品中16种苯系物[J].分析测试学报,2025,44(05):860-867. DOI: 10.12452/j.fxcsxb.241015468.
LU Duan-ping,CHENG Jia-hua,HONG Qing-ling,CHEN Xu,CHEN Shuo,JIAN Yu-ying,ZHENG Jing-feng,CHEN Zai-min.Determination of 16 Benzene Series in Sunscreen Cosmetics by Headspace-Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(05):860-867. DOI: 10.12452/j.fxcsxb.241015468.
该文基于顶空-气相色谱-质谱(HS-GC-MS),建立了防晒类化妆品中16种苯系物的分析方法。样品经甲醇分散后用水稀释,80 ℃平衡40 min,经HP-5MS毛细管色谱柱(30 m×0.25 mm×0.25 μm)分离,在GC-MS选择离子监测(SIM)模式下检测,以甲苯-D
8
和1,2-二氯苯-D
4
为内标,基质匹配标准曲线进行定量分析。结果显示,16种苯系物在相应的质量浓度范围内呈良好的线性关系(
r
≥0.997 4),检出限为0.02~0.06 μg∙g
-1
,两种基质在3个不同添加水平下的平均回收率为90.0%~103%,相对标准偏差(RSD)为0.20%~6.
5%。应用该方法对60批防晒类化妆品进行检测,有39批样品检出苯系物,其中间/对二甲苯、邻二甲苯、甲苯和乙苯的检出率较高,分别为45%、32%、16%、16%;5批防晒喷雾检出苯,含量均未超过《化妆品安全技术规范》(2015年版)规定的限值(2.0 mg∙kg
-1
),部分样品中邻二甲苯、1,3,5-三甲苯、间/对二甲苯的检出含量超过2.0 mg∙kg
-1
。该方法简便、快速、灵敏、准确,可用于防晒类化妆品中16种苯系物的含量测定。
In this study,a method for the detection of 16 benzene series in sunscreen cosmetics was established based on headspace-gas chromatography-mass spectrometry(HS-GC-MS). The samples were dispersed with methanol and diluted with water,then equilibrated at 80 ℃ for 40 min.The samples were separated on a HP-5MS capillary column(30 m×0.25 mm×0.25 μm),then detected by GC-MS in selected ion monitoring mode(SIM). Toluene-D
8
and 1,2-dichlorobenzene-D
4
were used as internal standards and matrix matching curves were used for quantitative analysis. The results showed good linearity(
r
≥0.997 4) for 16 benzene series in corresponding concentration ranges. The limits of detection were in the range of 0.02-0.06 μg∙g
-1
. The average recoveries of two substrates at three different spiked levels ranged from 90.0% to 103%,with the relative standard deviations(RSDs) ranged from 0.20% to 6.5%. The method was used to detect 60 batches of sunscreen cosmetics,benzene series were detected in 39 batches of samples,among which the detection rates of
m
-xylene
&
p
-xylene,
o
-xylene,toluene and ethylbenzene were 45%,32%,16% and 16%,respectively. Benzene was detected in five batches of sunscreen spray products,with content exceeding the limit(2.0 mg∙kg
-1
) in the
“Safety and Technical Standards for Cosmetics”
(
2015 edition
) . The content of
o
-xylene,1,3,5-tritylene and
m
-xylene
&
p
-xylene in some samples exceeded 2.0 mg∙kg
-1
. The method is simple,rapid,sensitive and accurate,which can be used for the determination of 16 benzene seri
es in sunscreen cosmetics.
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