15 chemical sunscreen agents in 220 batches of sun-proof products were tested,and the test results were checked with the product labels and approvals,and the problems found were compared and analyzed.There were some i...15 chemical sunscreen agents in 220 batches of sun-proof products were tested,and the test results were checked with the product labels and approvals,and the problems found were compared and analyzed.There were some inconsistencies among the actual ingredients,labeling ingredients and approval ingredients in the sun-proof products on the market,and the problem of insufficient input of raw materials was prominent.The supervision of this kind of products should be strengthened so as to reduce the safety risk of consumers using this kind of products.展开更多
建立了化妆品中包括乙基己基三嗪酮在内22种防晒剂的高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)确证方法。选择具有代表性的霜类和乳类基质的防晒化妆品作为研究对象。样品...建立了化妆品中包括乙基己基三嗪酮在内22种防晒剂的高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)确证方法。选择具有代表性的霜类和乳类基质的防晒化妆品作为研究对象。样品经过超声提取、过滤后,采用C_(18)色谱柱分离、电喷雾正离子源(ESI+)电离、多反应监测(MRM)模式扫描测定,确定了22种防晒剂的质谱确证离子对及质谱参数、流动相及梯度洗脱方法,得到的图谱峰型好,响应高。加标确证试验得出22种防晒剂的相对离子丰度比均在最大允许偏差范围内,相对离子丰度比的相对标准偏差(RSD)为0.4%~9.3%(n=10),出峰时间的RSD为0~0.5%(n=10)。该方法灵敏度高,准确性好,可用于化妆品中22种防晒剂的质谱确证分析,为实验室检测提供了技术支持,有助于化妆品防晒剂的质量监督。展开更多
选用CAPCELL PAK C18色谱柱为分离柱,柱温为30℃,进样体积为10.0μL,并用不同比例的(A)甲醇、(B)四氢呋喃和(C)0.008 2mol·L^-1高氯酸溶液的混合液作为流动相,按程序梯度洗脱模式对市售防晒产品中所用的15种防晒剂的标准品进行色...选用CAPCELL PAK C18色谱柱为分离柱,柱温为30℃,进样体积为10.0μL,并用不同比例的(A)甲醇、(B)四氢呋喃和(C)0.008 2mol·L^-1高氯酸溶液的混合液作为流动相,按程序梯度洗脱模式对市售防晒产品中所用的15种防晒剂的标准品进行色谱分离,并在波长311nm处进行紫外检测。实样分析时,称取样品0.25g,用甲醇、四氢呋喃、水和高氯酸(体积比为250∶450∶300∶0.2)的混合液(以下简称混合溶剂)15 mL超声提取30 min,用混合溶剂定容至25.0mL,离心10min,分取上清液1.0mL,加入混合溶剂定容至10.0mL,经0.45μm滤膜过滤,取滤液按仪器工作条件进行高效液相色谱分析。结果表明:所测定的15种防晒剂在一定的质量浓度范围内与其对应的峰面积呈线性关系。选定其中的二苯酮-3为参照物,并根据其余14种化合物的质量浓度和峰面积计算了各化合物的相对校正因子和相对保留时间等参数,确定了用一测多评法(QAMS)测定防晒产品中15种防晒剂的条件。还对色谱柱的型号、色谱仪器的型号以及柱温、进样量等对相对校正因子和保留时间可能产生影响的因素进行了系统试验。证明了在选定的色谱柱型号的前提下,用QAMS方法可实现防晒产品中15种防晒剂含量的同时测定。应用QAMS方法测定了6个批次防晒产品中的防晒剂含量,所得结果与用标准曲线法计算的结果基本一致,表明QAMS方法在降低检测成本和节省检测时间方面效果显著。展开更多
文摘15 chemical sunscreen agents in 220 batches of sun-proof products were tested,and the test results were checked with the product labels and approvals,and the problems found were compared and analyzed.There were some inconsistencies among the actual ingredients,labeling ingredients and approval ingredients in the sun-proof products on the market,and the problem of insufficient input of raw materials was prominent.The supervision of this kind of products should be strengthened so as to reduce the safety risk of consumers using this kind of products.
文摘建立了化妆品中包括乙基己基三嗪酮在内22种防晒剂的高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)确证方法。选择具有代表性的霜类和乳类基质的防晒化妆品作为研究对象。样品经过超声提取、过滤后,采用C_(18)色谱柱分离、电喷雾正离子源(ESI+)电离、多反应监测(MRM)模式扫描测定,确定了22种防晒剂的质谱确证离子对及质谱参数、流动相及梯度洗脱方法,得到的图谱峰型好,响应高。加标确证试验得出22种防晒剂的相对离子丰度比均在最大允许偏差范围内,相对离子丰度比的相对标准偏差(RSD)为0.4%~9.3%(n=10),出峰时间的RSD为0~0.5%(n=10)。该方法灵敏度高,准确性好,可用于化妆品中22种防晒剂的质谱确证分析,为实验室检测提供了技术支持,有助于化妆品防晒剂的质量监督。
基金supported by the National Key Research and Development Program of China(2018YFA0208702)the National Natural Science Foundation of China(No.22025304 and No.22033007)Guozhen Zhang is grateful for the start-up funding of University of Science and Technology of China.The numerical calculations in this work have been done in the Supercomputing Center of University of Science and Technology of China.
