一测多评方法应用于高效液相色谱法测定防晒产品中15种防晒剂的含量

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。

Application of the Analytical Mode of QAMS to HPLC Determination of 15 Sunscreen Agents in Sunscreen Cosmetics

CAPCELL PAK C18 chromatographic column,with column temperature of 30 ℃ and volume of sample introduction of 10.0μL,and mixtures of(A)methanol,(B)tetrahydrofuran,and(C)0.008 2 mol·L^-1 HClO4 solution in various ratios as mobile phases in gradient elution were selected for HPLC separation of standard for 15 sunscreen agents which were used frequently in preparation of sunscreen cosmetics.Ultraviolet detections at the wavelength of 311 nm were made for the determination of the 15 compounds.In analysis of substantial cosmetic sample,0.25 g of the sample was ultrasonically extracted with 15 mL of a mixed solvent of methanol,tetrahydrofuran,water and perchloric acid(250∶450∶300∶0.2 by vol.)for 30 min,and the volume of the extract was made up to 25.0 mL with the mixed solvent.After centrifugation,1.0 mL of the supernatant was taken,and diluted to 10.0 mL with the mixed solvent.The solution was then filtered through 0.45μm filtering membrane,and the filtrate was used for HPLC analysis according the working condtions of the instrument.It was shown that good linear relationships between values of peak areas of the 15 sunscreen agents found and their respective mass concentrations in definite ranges were obtained.Relative correction factors and relative retention times of 14 of the15 sunscreen agents were calculated from data of their mass concentrations and peak areas by taking diphenyl ketone-3 as reference.Based on these parameters,condition of analytical mode of QAMS as applied to the simultaneous HPLC determination of the 15 compounds in sunscreen cosmetics was established.Some factors,e.g.types of the chromatographic column and the chromatograph used,temperature of the LC column and volume of sample solution introduced that may effect the values of relative correction factors and relative retention times were also studied in detail.As shown by the testing results,when the qualified type of chromatographic column was chosen,the QAMS mode could be effectively used for the simultaneous determination of the 15 compounds.The proposed method was used in analysis of 6 samples from various batches,giving results in consistency with those given by the conventional method.Significant efficiency in saving of cost and time for analysis was shown by the mode of QAMS.