将超声辅助-分散液液微萃取(UA-DLLME)与气相色谱-质谱联用技术(GC-MS)相结合,建立了化妆品和化妆品模拟液中痕量增塑剂的检测方法.优化了前处理条件,并系统研究了模拟液种类、温度、时间对16种增塑剂迁移行为的影响.结果表明,化妆品属性对增塑剂的迁移行为有显著影响,脂溶性化妆品与塑料包装材料间的迁移情况较为严重;迁移量与温度、时间均呈正相关.在最佳萃取和检测条件下,该方法对16种增塑剂具有较高的富集倍数(88~106),在10~400 μg/L内呈良好的线性关系,相关系数R2为0.998 3~0.999 8,在3个加标质量浓度水平下的平均回收率为70.66%~99.65%,相对标准偏差为4.48%~14.56%,检出限为0.09~11.66 μg/L.该方法简捷、环保,可满足国际市场对增塑剂日趋严格的检测低限需求,为化妆品包装材料的选择提供实验依据.
A novel method of ultrasound-assisted dispersive liquid-liquid micro-extraction(UA-DLLME)was established for the detection of trace phthalates in cosmetic and cosmetic stimulants by gas chromatography-mass spectrometry(GC-MS). Pre-processing conditions were optimized. A systematic research was conducted to investigate the influence of the migration conditions(simulation, temperature and time)on the migration of 16 kinds of phthalates in cosmetics plastic packaging materials. It was proved that cosmetic properties had a significant effect on the migration. Under the optimal conditions, the proposed method provided higher enrichment factor(88~106), a good linearity(R2= 0.998 3~0.999 8)and the relative standard deviations(RSDs)were in the range of 4.48% ~ 14.56%. The limit of detection were within the scope of 0.09~11.66 μg/L. The satisfactory average recovery for 16 kinds of phthalates at three spiked levels ranged from 70.66% to 99.65%. This method was convenient, speedy, environmentally benign for detecting trace phthalates in cosmetics and cosmetic stimulants, which could meet the needs of international- DOI:10.3969/j.issn.1000-1565.2019.03.008化妆品塑料包装中16种增塑剂的迁移规律赵娜1,孙月娜2,时丽艳1,李攀2,吕运开2(1. 河北省产品质量监督检验研究院 基础检验部,河北 石家庄 050020;2.河北大学 化学与环境科学学院,河北 保定 071002)摘 要:将超声辅助-分散液液微萃取(UA-DLLME)与气相色谱-质谱联用技术(GC-MS)相结合,建立了化妆品和化妆品模拟液中痕量增塑剂的检测方法.优化了前处理条件,并系统研究了模拟液种类、温度、时间对16种增塑剂迁移行为的影响.结果表明,化妆品属性对增塑剂的迁移行为有显著影响,脂溶性化妆品与塑料包装材料间的迁移情况较为严重;迁移量与温度、时间均呈正相关.在最佳萃取和检测条件下,该方法对16种增塑剂具有较高的富集倍数(88~106),在10~400 μg/L内呈良好的线性关系,相关系数R2为0.998 3~0.999 8,在3个加标质量浓度水平下的平均回收率为70.66%~99.65%,相对标准偏差为4.48%~14.56%,检出限为0.09~11.66 μg/L.该方法简捷、环保,可满足国际市场对增塑剂日趋严格的检测低限需求,为化妆品包装材料的选择提供实验依据.关键词:气相色谱-质谱;超声辅助-分散液液微萃取;增塑剂;化妆品中图分类号:O657.1 文献标志码:A 文章编号:1000-1565(2019)03-0270-08Study on migration characteristic of 16 kinds of phthalates in cosmetic plastic packagesZHAO Na1, SUN Yuena1, SHI Liyan2, LI Pan2, LÜ Yunkai2(1.Foundation Inspection Department. Hebei Research Institution for Product Quality Supervision and Inspection, Shijiazhuang 050020, China; 2. College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China)Abstract:A novel method of ultrasound-assisted dispersive liquid-liquid micro-extraction(UA-DLLME)was established for the detection of trace phthalates in cosmetic and cosmetic stimulants by gas chromatography-mass spectrometry(GC-MS). Pre-processing conditions were optimized. A systematic research was conducted to investigate the influence of the migration conditions(simulation, temperature and time)on the migration of 16 kinds of phthalates in cosmetics plastic packaging materials. It was proved that cosmetic properties had a significant effect on the migration. Under the optimal conditions, the proposed method provided higher enrichment factor(88~106), a good linearity(R2= 0.998 3~0.999 8)and the relative standard deviations(RSDs)were in the range of 4.48% ~ 14.56%. The limit of detection were within the scope of 0.09~11.66 μg/L. The satisfactory average recovery for 16 kinds of phthalates at three spiked levels ranged from 70.66% to 99.65%. This method was convenient, speedy, environmentally benign for detecting trace phthalates in cosmetics and cosmetic stimulants, which could meet the needs of international- 收稿日期:2018-10-28 基金项目:河北省技术监督局科技计划项目(2014ZC05) 第一作者:赵娜(1984—),女,河北深泽人,工程师,主要从事产品质量检验.E-mail:zhaonasjz_1984@126.com 通信作者:李攀(1987—),女,河北永年人,河北大学实验师,主要从事色谱分析与食品安全分析.E-mail:hxxylp@hbu.edu.cn第3期赵娜等:化妆品塑料包装中16种增塑剂的迁移规律market for increasingly stringent requirements for detection limit. This research would provide experimental basis for the selection of packaging materials for different cosmetics.
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