Unilever R&D Shanghai, 66 Lin Xin Road, Linkong Economic Development Zone, Shanghai 200335, People's Republic of China; Analytical-Chemistry Group, Van't Hoff Institute for Molecular Sciences, University of Amsterdam, Science Park 904, 1098 XH Amsterdam, The Netherlands.
J Chromatogr A. 2013 Nov 22;1317:155-8. doi: 10.1016/j.chroma.2013.08.032. Epub 2013 Aug 13.
A sensitive and specific ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the measurement of climbazole deposition from hair care products onto artificial skin and human scalp. Deuterated climbazole was used as the internal standard. Atmospheric pressure chemical ionization (APCI) in positive mode was applied for the detection of climbazole. For quantification, multiple reaction monitoring (MRM) transition 293.0>69.0 was monitored for climbazole, and MRM transition 296.0>225.1 for the deuterated climbazole. The linear range ran from 4 to 2000 ng mL(-1). The limit of detection (LOD) and the limit of quantification (LOQ) were 1 ng mL(-1) and 4 ng mL(-1), respectively, which enabled quantification of climbazole on artificial skin and human scalp at ppb level (corresponding to 16 ng cm(-2)). For the sampling of climbazole from human scalp the buffer scrub method using a surfactant-modified phosphate buffered saline (PBS) solution was selected based on a performance comparison of tape stripping, the buffer scrub method and solvent extraction in in vitro studies. Using this method, climbazole deposition in in vitro and in vivo studies was successfully quantified.
建立并验证了一种用于测量护发产品中克霉唑在人工皮肤和人体头皮上沉积量的灵敏、特异的超高效液相色谱-串联质谱（UHPLC-MS/MS）法。以氘代克霉唑为内标，正离子大气压化学电离（APCI）模式进行检测。定量分析时，采用克霉唑的监测离子对 293.0>69.0 和内标物 296.0>225.1。克霉唑在 4~2000ng·mL(-1)浓度范围内线性良好。方法的检测限（LOD）和定量限（LOQ）分别为 1ng·mL(-1)和 4ng·mL(-1)，可实现在 ppb 水平（相当于 16ng·cm(-2)）对人工皮肤和人体头皮上的克霉唑进行定量分析。在体外研究中，通过对胶带撕脱法、缓冲液擦洗法和溶剂提取法的性能比较，选择了一种表面活性剂修饰的磷酸盐缓冲盐水（PBS）溶液的缓冲液擦洗法用于从人体头皮中采集克霉唑。使用该方法成功地对体外和体内研究中的克霉唑沉积量进行了定量分析。
