University of Chieti-Pescara "G. d'Annunzio", Department of Pharmacy, Chieti, Italy.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Jun 15;1118-1119:40-50. doi: 10.1016/j.jchromb.2019.04.028. Epub 2019 Apr 16.
This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-photodiode array detection (FPSE-HPLC-PDA) method for the simultaneous extraction and analysis of six benzophenone derivative UV filters including benzophenone (BZ); 5-benzoyl-4-hydroxy-methoxybenzenesulfonic acid (BP-4); bis(4-hydroxyphenyl)methanone (4-DHB); bis(2,4-dihydroxyphenyl)methanone (BP-2); (2,4-dihydroxybenzophenone) (BP-1) and 2,2'-dihydroxy-4-methoxybenzophenone (DHMB) in human whole blood, plasma and urine samples. Chromatographic separation method was conducted using a Spherisorb ODS 1 (C) column in isocratic elution mode with a run time <25 min. The FPSE-HPLC-PDA method was validated in the range from 0.1 to 10 μg/mL for all the UV filter compounds. Propyl 4-hydroxybenzoate (also known as propyl paraben) was used as the internal standard (IS). The limit of quantification was found to be 0.1 μg/mL and the weighted-matrix matched standard calibration curves of six UV filters showed a good linearity up to a concentration of 10 μg/mL. This new approach exhibits high potential for direct adaptation as a rapid, robust and green analytical tool for several applications, e.g. in the current sample preparation practices used in many bioanalytical fields including pharmacokinetics (PK), pharmacodynamics (PD), therapeutic drug monitoring (TDM), clinical and forensic toxicology, disease diagnosis and drug discovery. Additionally, in the present work was highlighted that applying innovative extraction and clean up procedures before instrumental analysis by means of a well-known, rugged, cheap, and diffused configurations (e.g. HPLC-PDA), could be possible to validate methods that shows analytical performances comparable to more expensive and complex instrumentations (e.g. LC-MS/MS) that require trained personnel, high maintenance costs and a deep knowledge of analytical problems that could be encountered.
本文报道了一种新颖的纤维状相固相萃取-高效液相色谱-光电二极管阵列检测（FPSE-HPLC-PDA）方法，用于同时提取和分析 6 种二苯甲酮衍生物紫外线滤光剂，包括二苯甲酮（BZ）、5-苯甲酰基-4-羟基甲氧基苯磺酸（BP-4）、双（4-羟基苯基）甲烷（4-DHB）、双（2,4-二羟基苯基）甲烷（BP-2）、（2,4-二羟基二苯甲酮）（BP-1）和 2,2'-二羟基-4-甲氧基二苯甲酮（DHMB）在人全血、血浆和尿液样本中的含量。色谱分离方法采用 Spherisorb ODS 1（C）柱，在等度洗脱模式下运行时间<25min。FPSE-HPLC-PDA 方法在所有紫外线滤光剂化合物的 0.1 至 10μg/mL 范围内进行了验证。丙酸 4-羟基苯甲酸酯（也称为丙酸对羟基苯甲酸酯）用作内标（IS）。定量限为 0.1μg/mL，6 种紫外线滤光剂的加权基质匹配标准校准曲线在 10μg/mL 浓度范围内表现出良好的线性关系。这种新方法具有直接适应快速、稳健和绿色分析工具的高潜力，例如在当前许多生物分析领域（包括药代动力学（PK）、药效动力学（PD）、治疗药物监测（TDM）、临床和法医毒理学、疾病诊断和药物发现）中使用的样品制备实践。此外，在本工作中强调，通过使用众所周知的、坚固的、廉价的和广泛应用的配置（例如 HPLC-PDA），在仪器分析之前应用创新的提取和净化程序，有可能验证分析性能与更昂贵和复杂的仪器（例如 LC-MS/MS）相当的方法，这些仪器需要经过培训的人员、高维护成本以及对可能遇到的分析问题的深入了解。
