Dipartimento di Scienza e Tecnologia del Farmaco, Università degli Studi di Torino, Via P. Giuria 9, I-10125 Torino, Italy.
J Chromatogr A. 2010 Apr 16;1217(16):2599-605. doi: 10.1016/j.chroma.2009.12.052. Epub 2010 Jan 4.
This study describes a method based on direct contact sorptive tape extraction followed by on-line thermal desorption gas chromatography-mass spectrometry (DC-STE-GC-MS) to detect and quantify a group of suspected volatile allergens on the European Union (E.U.) list and a related compound on the skin (the stratum corneum) of volunteers treated with a cream of known composition fortified with the reference allergens. The following compounds were tested: citronellol, Z-citral (neral), geraniol, cinnamaldehyde, anisyl alcohol, cinnamyl alcohol, eugenol, methyleugenol, coumarin, isoeugenol, alpha-isomethylionone, 2-(4-tert-butylbenzyl)propionaldehyde (lilial), alpha-amylcinnamaldehyde, alpha-hexylcinnamaldehyde. Sorptive tape extraction (STE) is a sorption-based sampling technique in which a flexible polydimethylsiloxane (PDMS) tape is used to recover analytes by direct contact with the surface of a solid matrix or from the headspace in equilibrium with it. The reliability of the method was confirmed by: (i) allergen recoveries varying from 52.3% for lilial to 95.7% for neral, (ii) linearity in the range 10-150ppm, with regression coefficient R(2) always above 0.97, (iii) repeatability of each analyte, RSD% never exceeding 10%, (iv) intermediate precision, always below 15%, and (v) LOD and LOQ in the ppb range, therefore fully compatible with E.U. prescriptions (ppm). Other parameters such as substantivity analyte, approximate permeation through skin and influence of different nature of stratum corneum on recovery were also investigated. The method was also successfully applied to five commercially available creams declared to contain some of the allergens in question spread on the skin of the same volunteers.
本研究描述了一种基于直接接触吸附带提取(DC-STE),然后在线热解吸气相色谱-质谱联用(GC-MS)的方法,用于检测和量化欧盟(EU)清单上一组疑似挥发性过敏原,以及一种相关化合物在使用已知成分乳膏处理的志愿者皮肤上的含量,该乳膏中添加了参考过敏原。测试了以下化合物:香茅醇、Z-柠檬醛(橙花醛)、香叶醇、肉桂醛、苯甲醇、肉桂醇、丁香酚、甲基丁香酚、香豆素、异丁香酚、α-异甲基紫罗兰酮、2-(4-叔丁基苄基)丙醛(Lilial)、α-戊基肉桂醛、α-己基肉桂醛。吸附带提取(STE)是一种基于吸附的采样技术,其中使用柔性聚二甲基硅氧烷(PDMS)带通过与固体基质表面直接接触或与其平衡的顶空来回收分析物。该方法的可靠性通过以下几个方面得到了确认:(i)Lilial 的回收率从 52.3%到橙花醛的 95.7%不等,(ii)10-150ppm 范围内的线性关系,回归系数 R²始终高于 0.97,(iii)每个分析物的重复性,RSD%从不超过 10%,(iv)中间精度,始终低于 15%,以及(v)LOD 和 LOQ 在 ppb 范围内,因此完全符合欧盟规定(ppm)。还研究了其他参数,如分析物的持久性、近似透过皮肤的渗透率以及不同性质的角质层对回收率的影响。该方法还成功应用于五种市售乳膏,这些乳膏宣称含有一些涂在同一志愿者皮肤上的可疑过敏原。