Vela-Soria F, Ballesteros O, Zafra-Gómez A, Ballesteros L, Navalón A
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
Talanta. 2014 Apr;121:97-104. doi: 10.1016/j.talanta.2013.12.048. Epub 2013 Dec 30.
Benzophenone-UV filters (BP-UV filters) are extensively used in cosmetics products to avoid damaging effects of UV radiation. Despite their low toxicity, many research papers indicate that BP-UV filters are weak endocrine disruptors (EDCs). There are clear relationships between BP-UV filters exposure and several health disorders such as carcinogenesis and malformations observed in animals. In the present work, a new sample treatment procedure by dispersive liquid-liquid microextraction (DLLME) is proposed for the extraction of six BPs, namely benzophenone-1 (BP-1), benzophenone-2 (BP-2), benzophenone-3 (BP-3), benzophenone-6 (BP-6), benzophenone-8 (BP-8) and 4-hydroxybenzophenone (4-OH-BP), in human serum samples, followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis. The method involves an enzymatic treatment to quantify the total content (free plus conjugated species) of BP-UV filters in serum. The extraction parameters were accurately optimized using multivariate optimization approach. Benzophenone-d₁₀ (BP-d₁₀) was used as surrogate. Limits of quantification (LOQs) ranged from 0.4 to 0.9 ng mL(-1) and inter-day precision (evaluated as relative standard deviation) ranged from 1.9% to 13.1%. The method was validated using matrix-matched calibration and a recovery assay. Recovery rates for spiked samples ranged from 97% to 106%, and acceptable linearity was obtained up to concentrations of 40 ng mL(-1). The method was applied to the determination of the target compounds in human serum samples from 20 randomly selected anonymous individuals.
二苯甲酮类紫外线过滤剂（BP-UV过滤剂）被广泛用于化妆品中，以避免紫外线辐射的有害影响。尽管其毒性较低，但许多研究论文表明，BP-UV过滤剂是弱内分泌干扰物（EDC）。在动物身上观察到，接触BP-UV过滤剂与几种健康问题之间存在明确的关系，如致癌作用和畸形。在本研究中，提出了一种通过分散液液微萃取（DLLME）的新型样品处理程序，用于萃取人血清样品中的六种二苯甲酮，即二苯甲酮-1（BP-1）、二苯甲酮-2（BP-2）、二苯甲酮-3（BP-3）、二苯甲酮-6（BP-6）、二苯甲酮-8（BP-8）和4-羟基二苯甲酮（4-OH-BP），随后进行超高效液相色谱-串联质谱（UPLC-MS/MS）分析。该方法涉及酶处理，以定量血清中BP-UV过滤剂的总含量（游离和结合形式）。使用多变量优化方法精确优化了萃取参数。二苯甲酮-d₁₀（BP-d₁₀）用作替代物。定量限（LOQ）范围为0.4至0.9 ng mL⁻¹，日间精密度（以相对标准偏差评估）范围为1.9%至13.1%。该方法通过基质匹配校准和回收率测定进行了验证。加标样品的回收率范围为97%至106%，在浓度高达40 ng mL⁻¹时获得了可接受的线性。该方法应用于20名随机选择的匿名个体的人血清样品中目标化合物的测定。
