Guangzhou Key Laboratory of Subtropical Biodiversity and Biomonitoring and Guangdong Provincial Engineering Technology Research Center for Drug and Food Biological Resources Processing and Comprehensive Utilization, School of Life Sciences, South China Normal University, Guangzhou 510631, China.
Guangzhou Key Laboratory of Subtropical Biodiversity and Biomonitoring and Guangdong Provincial Engineering Technology Research Center for Drug and Food Biological Resources Processing and Comprehensive Utilization, School of Life Sciences, South China Normal University, Guangzhou 510631, China; Guangxi Zhuang Autonomous Region Institute of Product Quality Inspection, Nanning 530000, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Apr 15;1237:124090. doi: 10.1016/j.jchromb.2024.124090. Epub 2024 Mar 20.
Accurate monitoring of UV-filters exposure levels in human plasma is a challenge because of the significant differences in the physicochemical properties of UV-filters, as well as the matrix effect caused by abundant proteins and phospholipids in plasma. Therefore, an effective and rapid method for simultaneous determination of 14 UV-filters in human plasma using protein precipitation-solid phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed. Acetonitrile with 0.1 % formic acid and 10 % isopropanol (v/v) were used as mobile phases. A gradient elution on an ACQUITY UPLC BEH-C18 column at 30 °C and 0.3 mL/min flow rate was applied for separation. The electrospray ionization positive or negative modes were selected to determine the corresponding analyte to increase selectivity and sensitivity. Results showed that acetonitrile-tetrahydrofuran (v/v, 8:2) as the extraction solvent can effectively precipitate protein in plasma and improve the solubility of UV-filters. The HybridSPE cartridge improved the removal efficiency of phospholipids, while 1 mL of methanol elution increased the extraction recoveries of targets. Fourteen UV-filters achieved good linearities, low detection limits (0.050 to 0.10 μg/L) and quantification limits (0.10 to 1.0 μg/L). Method accuracy and precision, extraction recoveries, and storage stabilities of all analytes met the criterion of 80-120 %. Moreover, this method was successfully applied for the determination of UV-filters in plasma randomly collected from adults. Nine of 14 UV-filters were determined and their concentrations were distributed widely, suggesting a big variation of individual UV-filters exposure.
准确监测人体血浆中紫外线滤光剂的暴露水平是一项挑战，这是由于紫外线滤光剂的物理化学性质存在显著差异，以及血浆中丰富的蛋白质和磷脂所造成的基质效应。因此，建立了一种使用蛋白质沉淀-固相萃取（SPE）与液相色谱串联质谱（LC-MS/MS）相结合的有效、快速的方法，用于同时测定人血浆中的 14 种紫外线滤光剂。乙腈中含 0.1%甲酸和 10%异丙醇（v/v）作为流动相。在 30°C 和 0.3mL/min 的流速下，在 ACQUITY UPLC BEH-C18 柱上进行梯度洗脱，以提高选择性和灵敏度。选择电喷雾电离正或负离子模式来测定相应的分析物。结果表明，乙腈-四氢呋喃（v/v，8:2）作为提取溶剂可以有效地沉淀血浆中的蛋白质，提高紫外线滤光剂的溶解度。混合 SPE 萃取小柱提高了磷脂的去除效率，而 1mL 甲醇洗脱增加了目标物的提取回收率。14 种紫外线滤光剂均具有良好的线性、低检测限（0.050-0.10μg/L）和定量限（0.10-1.0μg/L）。所有分析物的方法准确度和精密度、提取回收率和储存稳定性均符合 80%-120%的标准。此外，该方法成功应用于测定成人随机采集的血浆中的紫外线滤光剂。确定了 14 种紫外线滤光剂中的 9 种，其浓度分布广泛，表明个体紫外线滤光剂暴露存在较大差异。
