用于测定防晒配方中四种化学紫外线过滤剂的非水反相高效液相色谱法的建立与验证

Development and validation of a non-aqueous reversed-phase high-performance liquid chromatographic method for the determination of four chemical UV filters in suncare formulations.

作者信息

Smyrniotakis C G, Archontaki Helen A

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis, Athens 15771, Greece.

出版信息

J Chromatogr A. 2004 Mar 26;1031(1-2):319-24. doi: 10.1016/j.chroma.2003.08.078.

DOI:10.1016/j.chroma.2003.08.078

PMID:15058600

Abstract

A non-aqueous reversed-phase high performance liquid chromatographic method (RP-HPLC) with UV detection at 313 nm was developed and validated for simultaneous determination of methylene bis-benzotriazolyl tetramethylphenol (Tinosorb M) along with three other chemical UV filters, octocrylene (Eusolex OCR), octyl methoxycinnamate (Eusolex 2292) and octyl salicylate (Eusolex OS) in suncare products. An isocratic elution was performed on a Hypersil BDS RP-C18 column (250 mm x 4.6 mm), 5 microm particle size, using a mobile phase consisted of methanol-acetonitrile (90:10, v/v) with a flow-rate of 1.5 ml/min. The determination of the four UV filters was not interfered by the excipients in the products. The method of external standard, as well as the standard addition method was used for the determination. The external standard calibration curves were linear for Eusolex OCR, Eusolex 2292, Eusolex OS, and Tinosorb M in the concentration ranges of 0.5-100 microM, 0.5-100 microM, 0.5-200 microM, and 0.2-100 microM, respectively. Day-to-day relative standard deviation of the determination was within 3%. Limits of detection and quantitation of the above compounds were found equal to 36 and 110 nM, 220 and 660 nM, 170 and 520 nM, 44 and 130 nM, respectively. The recovery of these four chemical UV filters from the spiked samples was 96-103%.

摘要

建立了一种非水反相高效液相色谱法（RP-HPLC），该方法在313 nm处进行紫外检测，用于同时测定防晒产品中的亚甲基双苯并三唑基四甲基苯酚（Tinosorb M）以及其他三种化学紫外线过滤剂，即二乙氨羟苯甲酰基苯甲酸己酯（Eusolex OCR）、甲氧基肉桂酸辛酯（Eusolex 2292）和水杨酸辛酯（Eusolex OS）。在粒径为5微米的Hypersil BDS RP-C18柱（250 mm×4.6 mm）上进行等度洗脱，流动相为甲醇-乙腈（90:10，v/v），流速为1.5 ml/min。产品中的辅料不干扰这四种紫外线过滤剂的测定。采用外标法和标准加入法进行测定。外标校准曲线在以下浓度范围内呈线性：Eusolex OCR为0.5-100 microM，Eusolex 2292为0.5-100 microM，Eusolex OS为0.5-200 microM，Tinosorb M为0.2-100 microM。测定的日常相对标准偏差在3%以内。上述化合物的检测限和定量限分别为36和110 nM、220和660 nM、170和520 nM、44和130 nM。加标样品中这四种化学紫外线过滤剂的回收率为96-103%。