作者：张玉霞, 李丹, 林洁, 康天怿, 陈芙蓉, 宁欣, 徐小平
作者单位：四川大学华西药学院, 四川 成都 610041
关键词：毛细管GC;二羟二丁基醚;手性杂质;含量测定
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 m0.53 mm1.0 m)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 g/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。
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
2015, 41(12): 41-44 收稿日期: 2015-03-20;收到修改稿日期: 2015-05-07
基金项目:
作者简介: 张玉霞(1990-),女,四川绵阳市人,硕士研究生,专业方向为药物质量控制与药物代谢分析。
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