摘  要：采用毛细管气相色谱法（CGC）分别对二羟二丁基醚（DHDB）及手性杂质的分离条件进行考察，建立二羟二丁基醚（DHDB）含量的测定方法。PEG-20M（30 m×0.53 mm×1.0 μm）毛细管柱为色谱柱，FID为检测器，正辛醇作为内标，DHDB手性杂质程序升温条件为初温120 ℃，以0.5 ℃/min升温至180 ℃，保持40 min；DHDB含量测定程序升温条件为140 ℃保持1 min，以20 ℃/min升至200 ℃。DHDB及其手性异构体得到完全分离；DHDB在66.70~800.1 μg/mL的范围具有良好的线性关系（y=0.007 0x+0.055 4；r2=0.999 6）；平均回收率为99.54%，重复性RSD为0.68%，中间精密度RSD为0.95%，样品的平均含量为77.92%（RSD=0.25%）。该方法快速、简便，适于DHDB手性杂质分析和含量测定。

关键词：毛细管GC；二羟二丁基醚；手性杂质；含量测定

文献标志码：A       文章编号：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