摘要
建立化妆品中Cr(Ⅵ)的高效液相色谱–电感耦合等离子体质谱(HPLC-ICP-MS)分析方法.样品使用0.5mol/L氢氧化钠–0.28 mol/L无水碳酸钠–磷酸盐缓冲液涡旋超声提取后离心,以56 mmol/L硝酸–80 mmol/L氨水(pH=9.4,用氨水调节)为流动相,经阴离子色谱柱Hamilton PRP-X100 (250 mm×4.1 mm,10μm)分离,ICP-MS进行测定.在优化的测试条件下,Cr(Ⅵ)在0~50μg/L范围内线性关系良好,相关系数r≥0.999. Cr(Ⅵ)的检出限(LOD)为0.006 5 mg/kg,定量限(LOQ)为0.021 mg/kg,样品的加标回收率为85.0%~97.0%,相对标准偏差(RSD)为0.9%~6.9%.在不同基质的实际化妆品样品中检出了Cr(Ⅵ),重现性好,灵敏度高,并且碱性提取液对样品中的Cr(Ⅵ)提取相对完全,在氯化镁的辅助下Cr(Ⅵ)较稳定,所以适用于不同基质化妆品中Cr(Ⅵ)的检测.
A method for the determination of Cr(Ⅵ)in cosmetics by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)has been established.The samples were extracted using a 0.5 mol/L sodium hydroxide-0.28 mol/L anhydrous sodium bicarbonate-phosphate buffer solution through vortex ultrasonication followed by centrifugation.The mobile phase was 56 mmol/L nitric acid-80 mmol/L ammonia(pH=9.4,adjusted by ammonia).The samples were separated on a Hamilton PRP-X100(250 mm×4.1 mm,10µm)anionic column and determined by ICP-MS.Under the optimized conditions,Cr(Ⅵ)had a good linear relationship in the range of 0~50μg/L,and the correlation coefficient was r≥0.999.The limit of detection(LOD)of Cr(Ⅵ)was 0.0065 mg/kg,the limit of quantitation(LOQ)was 0.021 mg/kg,the spiked recoveries of samples were 85.0%~97.0%,and the relative standard deviations(RSD)were 0.9%~6.9%.Cr(Ⅵ)was detected in cosmetic samples with different matrices with good reproducibility and sensitivity.The extraction of Cr(Ⅵ)from the samples was more complete with the alkaline extraction solution,and the extraction of Cr(Ⅵ)was more stable with the assistance of magnesium chloride,so the method is suitable for the determination of Cr(Ⅵ)in cosmetics with different matrices.
作者
徐勤科
李若琦
魏学冰
郭朝晖
孙莺
雷虹
XU Qinke;LI Ruoqi;WEI Xuebing;GUO Zhaohui;SUN Ying;LEI Hong(Gansu Institute of Drug Control,Lanzhou 730070,China)
出处
《分析测试技术与仪器》
CAS
2024年第6期366-371,共6页
Analysis and Testing Technology and Instruments
基金
甘肃省药品监督管理局科研项目(2023GSMPA066)。
