Dohta Yukifumi, Yamashita Taro, Horiike Satomi, Nakamura Tatsuji, Fukami Takehiro
Tsukuba Research Institute, Banyu Pharmaceutical Co., Ltd., 3 Okubo, Tsukuba, Ibaraki 300-2611, Japan.
Anal Chem. 2007 Nov 1;79(21):8312-5. doi: 10.1021/ac0709798. Epub 2007 Oct 2.
A system for screening of the octanol/water distribution coefficient (LogD) using automatic sampling of 96-well plates was developed. The high-speed assay for LogD (HSLogD) screening uses a water-plug aspiration/injection method combined with high-performance liquid chromatography-mass spectrometry (HPLC-MS). The method is useful for LogD analysis of highly hydrophobic compounds, where the concentration of the compound in the octanol phase is much higher than that in the water phase. In the case of LogD analyses, the conventional shake-flask method has been widely used, but it is difficult to increase the throughput of the shake-flask method because the lower water phase is carefully separated by manual separation without contamination of the upper octanol phase. We attempted to develop an automatic sampling method instead of manual separation to increase the throughput of the measurement. In initial attempts at automatic sampling, contamination of the octanol phase occurred when sampling of the water phase was made. This was because the octanol phase entered the sampling needle as it passed through to the lower water phase. This contamination was prevented by taking up a few microliters of water into the needle as a plug before sampling of the water phase (the water-plug aspiration/injection method). LogD values of some common drugs measured using the HSLogD agreed with reported LogD values (0 < LogD < 5).
开发了一种使用96孔板自动进样来筛选正辛醇/水分配系数(LogD)的系统。LogD的高速测定法(HSLogD)筛选采用水塞进样/注射法结合高效液相色谱-质谱联用(HPLC-MS)。该方法对于高疏水性化合物的LogD分析很有用,这类化合物在正辛醇相中的浓度远高于水相中的浓度。在LogD分析中,传统的摇瓶法已被广泛使用,但由于需要人工小心分离下层水相且不污染上层正辛醇相,因此难以提高摇瓶法的通量。我们试图开发一种自动进样方法来替代人工分离,以提高测量通量。在自动进样的初步尝试中,对水相进行采样时出现了正辛醇相污染的情况。这是因为正辛醇相在采样针穿过进入下层水相时进入了采样针。通过在对水相进行采样之前在针中吸取几微升水作为塞子(水塞进样/注射法),可防止这种污染。使用HSLogD测定的一些常用药物的LogD值与报道的LogD值(0 < LogD < 5)相符。