摘 要：采用毛細(xì)管氣相色譜法（CGC）分別對(duì)二羥二丁基醚（DHDB）及手性雜質(zhì)的分離條件進(jìn)行考察，建立二羥二丁基醚（DHDB）含量的測(cè)定方法。PEG-20M（30 m×0.53 mm×1.0 μm）毛細(xì)管柱為色譜柱，F(xiàn)ID為檢測(cè)器，正辛醇作為內(nèi)標(biāo)，DHDB手性雜質(zhì)程序升溫條件為初溫120 ℃，以0.5 ℃/min升溫至180 ℃，保持40 min；DHDB含量測(cè)定程序升溫條件為140 ℃保持1 min，以20 ℃/min升至200 ℃。DHDB及其手性異構(gòu)體得到完全分離；DHDB在66.70~800.1 μg/mL的范圍具有良好的線性關(guān)系（y=0.007 0x+0.055 4；r2=0.999 6）；平均回收率為99.54%，重復(fù)性RSD為0.68%，中間精密度RSD為0.95%，樣品的平均含量為77.92%（RSD=0.25%）。該方法快速、簡(jiǎn)便，適于DHDB手性雜質(zhì)分析和含量測(cè)定。
關(guān)鍵詞：毛細(xì)管GC；二羥二丁基醚；手性雜質(zhì)；含量測(cè)定
文獻(xiàn)標(biāo)志碼：A 文章編號(hào)：1674-5124（2015）12-0041-04
CGC separation of DHDB and chiral impurities
ZHANG Yuxia， LI Dan， LIN Jie， KANG Tianyi， CHEN Furong， NING Xin， XU Xiaoping
（School of Pharmacy，Sichuan University，Chengdu 610041，China）
Abstract: Capillary Gas Chromatography（CGC） has been adopted to determine the content of dihydroxydibutylether（DHDB） based on the separation conditions of DHDB and its chiral impurities. Chromatographic column：PEG-20M capillary column （30 m×0.53 mm×1.0 μm）； detector: flame ionization detector （FID）； internal standard （IS）：n-Octano. The separation conditions of DHDB and its chiral impurities are as follows：The column temperature was programmed from 120 ℃ to 180 ℃ at the rate of 0.5 ℃/min and then stayed there for 40 min. The assaying conditions of DHDB are as follows：The column temperature stayed at 140 ℃ for one minute and then programmed to 200 ℃ at the rate of 20 ℃/min. DHDB and its chiral impurities have been completely separated. The liner relationship of DHDB is good within the range of 66.70 μg/mL to 800.1 μg/mL（y=0.007 0x+0.055 4； r2=0.999 6）. The average recovery， repeatability RSD， intermediate precision RSD and mean content are 99.54%， 0.68%， 0.95% and 77.92% （RSD=0.25%） respectively. The two chromatographic conditions established are suitable for separating DHDB from its chiral impurities and determining the content of DHDB. It is convenient， fast and practical.
Keywords: CGC； dihydroxydibutylether； chiral impurities； content detecting
