顶空气相色谱法测定替考拉宁纯化中10种树脂残留溶剂
|
摘要
采用顶空气相色谱法,色谱柱为DB-FFAP毛细管柱,顶空平衡温度为85℃,平衡时间为40min,通过程序升温测定了替考拉宁纯化中10种大孔树脂残留溶剂。结果表明,在0.06～1.20μg·mL-1范围内,正己烷、氯苯和二乙烯苯的峰面积与浓度线性关系良好(R分别为0.997 6、0.996 8、0.996 8),平均回收率分别为101.25%、100.84%、101.03%;在0.12～2.40μg·mL-1范围内,丙烯酸乙酯、甲基丙烯酸甲酯、甲苯、二甲苯和苯乙烯线性关系良好(R分别为0.999 9、0.996 2、0.996 8、0.996 9、0.996 8),平均回收率分别为101.38%、101.20%、100.93%、100.87%、100.76%;在0.012～0.240μg·mL-1范围内,苯和1,2-二氯乙烷线性关系良好(R分别为0.996 6、0.996 2),平均回收率分别为101.29%、102.16%。该方法操作简单、准确度高、重复性好,可用于替考拉宁树脂残留物的质量控制。
We determined ten residual solvents of macroporous adsorbent resin in the purification of Teicoplanin by headspace gas chromatography under the conditions as follows:using DB-FFAP capillary column,at the headspace equilibrium temperature of 85℃,for the headspace equilibrium time of 40 min,and using temperature programming.The results show that the calibration curves of hexyl hydride,chlorobenzene,and diethylene benzene show good linear relationship within the range of 0.06-1.20μg·mL-1(R=0.997 6,0.996 8,0.9968),and the average recoveries are 101.25%,100.84%,and 101.03%,respectively.Moreover,the calibration curves of ethyl acrylate,methacrylate,methylbenzene,xylene,and styrene show good linear relationship within the range of 0.12-2.40μg·mL-1(R=0.999 9,0.996 2,0.996 8,0.996 9,0.996 8),and the average recoveries are 101.38%,101.20%,100.93%,100.87%,and 100.76%,respectively.Furthermore,benzene and 1,2-dichloroethane have good linear relationship within the range of 0.012-0.240μg·mL-1(R=0.996 6,0.996 2),andthe average recoveries are 101.29%and 102.16%,respectively.The method is simple,accurate,and repetitive,which can be used to control the resin residues in Teicoplanin.
We determined ten residual solvents of macroporous adsorbent resin in the purification of Teicoplanin by headspace gas chromatography under the conditions as follows:using DB-FFAP capillary column,at the headspace equilibrium temperature of 85℃,for the headspace equilibrium time of 40 min,and using temperature programming.The results show that the calibration curves of hexyl hydride,chlorobenzene,and diethylene benzene show good linear relationship within the range of 0.06-1.20μg·mL-1(R=0.997 6,0.996 8,0.9968),and the average recoveries are 101.25%,100.84%,and 101.03%,respectively.Moreover,the calibration curves of ethyl acrylate,methacrylate,methylbenzene,xylene,and styrene show good linear relationship within the range of 0.12-2.40μg·mL-1(R=0.999 9,0.996 2,0.996 8,0.996 9,0.996 8),and the average recoveries are 101.38%,101.20%,100.93%,100.87%,and 100.76%,respectively.Furthermore,benzene and 1,2-dichloroethane have good linear relationship within the range of 0.012-0.240μg·mL-1(R=0.996 6,0.996 2),andthe average recoveries are 101.29%and 102.16%,respectively.The method is simple,accurate,and repetitive,which can be used to control the resin residues in Teicoplanin.
引文
[1] PARENTI F,BERETTA G,BERTI M,et al.Teichomycins,new antibiotics from Actinoplanes teichomyceticus Nov.sp.Ⅰ.description of the producer stain,fermentation studies and biologial properties[J].The Journal of Antibiotics,1978,31(4):276-283.
[2]陆鹏,吴宝发,何聪,等.替考拉宁与万古霉素治疗革兰阳性菌感染的临床研究[J].中华医学感染学杂志,2018,28(2):173-176.LU P,WU B F,HE C,et al.Clinical effects of Teicoplanin and vancomycin on treatment of gram-positive bacteria infections[J].Chinese Journal of Nosocomiology,2018,28(2):173-176.
[3]周战云,郭月玲,耿艳辉,等.替考拉宁吸附树脂的筛选[J].河北化工,2007,30(3):18-23.ZHOU Z Y,GUO Y L,GENG Y H,et al.The sieve of adsorptive resins in Teicoplanin[J].Hebei Chemical Engineering and Industry,2007,30(3):18-23.
[4]耿文飞,吴军营,王春霞,等.顶空气相色谱法测定替考拉宁原料药及注射剂中5种有机溶剂残留量[J].中国药房,2015,26(18):2554-2556.GANG W F,WU J Y,WANG C X,et al.Determination of residues of 5organic solvents in Teicoplanin raw material and injection by headspace GC[J].China Pharmacy,2015,26(18):2554-2556.
[5]审评一部.再谈大孔树脂[EB/OL],http://www.cde.org.cn/dzkw.do?id=1259&method=largePage 20030729.
[6] GB/T 24396―2009.食品工业用吸附树脂产品测定方法[S].
[7]宋丹,张永文.试谈中药提取工艺中使用大孔吸附树脂纯化的研究要求与评价[J].中国新药杂志,2015,24(7):745-749.SONG D,ZHANG Y W.Requirement and evaluation of studies on using macroporous adsorption resin for further purification of extracts from Chinese herbal medicines[J].Chinese Journal of New Drugs,2015,24(7):745-749.
[8]申桃.丙烯酸树脂及其复合材料的制备与性能研究[D].成都:电子科技大学,2017.SHEN T.Preparation and study on the properties of acrylic resin and acrylic composites[D].Chengdu:University of Electronic Science and Technology of China,2017.
[9]曾文雪,涂瑶生,王金钱,等.GC测定AB-8树脂中有机残留物间二乙烯苯和对二乙烯苯的含量[J].时珍国医国药,2013,24(4):802-803.ZENG W X,TU Y S,WANG J Q,et al.Determination organic residuum of 1,3-divinylbenzene and 1,4-divinylbenzene in macroporous resin by GC[J].Lishizhen Med Mater Med Res,2013,24(4):802-803.
[10]孙悦,王卫,唐素芳.顶空气相色谱法测定盐酸帕罗西汀中残留的有机溶剂及基质效应考察[J].药物分析杂志,2010,30(5):963-967.SUN Y,WANG W,TANG S F.Determination of residual organic solvents in paroxetine hydrochloride by headspace capillary GC and research of matrix-induced effect[J].Chinese Journal of Pharmaceutical Analysis,2010,30(5):963-967.
[2]陆鹏,吴宝发,何聪,等.替考拉宁与万古霉素治疗革兰阳性菌感染的临床研究[J].中华医学感染学杂志,2018,28(2):173-176.LU P,WU B F,HE C,et al.Clinical effects of Teicoplanin and vancomycin on treatment of gram-positive bacteria infections[J].Chinese Journal of Nosocomiology,2018,28(2):173-176.
[3]周战云,郭月玲,耿艳辉,等.替考拉宁吸附树脂的筛选[J].河北化工,2007,30(3):18-23.ZHOU Z Y,GUO Y L,GENG Y H,et al.The sieve of adsorptive resins in Teicoplanin[J].Hebei Chemical Engineering and Industry,2007,30(3):18-23.
[4]耿文飞,吴军营,王春霞,等.顶空气相色谱法测定替考拉宁原料药及注射剂中5种有机溶剂残留量[J].中国药房,2015,26(18):2554-2556.GANG W F,WU J Y,WANG C X,et al.Determination of residues of 5organic solvents in Teicoplanin raw material and injection by headspace GC[J].China Pharmacy,2015,26(18):2554-2556.
[5]审评一部.再谈大孔树脂[EB/OL],http://www.cde.org.cn/dzkw.do?id=1259&method=largePage 20030729.
[6] GB/T 24396―2009.食品工业用吸附树脂产品测定方法[S].
[7]宋丹,张永文.试谈中药提取工艺中使用大孔吸附树脂纯化的研究要求与评价[J].中国新药杂志,2015,24(7):745-749.SONG D,ZHANG Y W.Requirement and evaluation of studies on using macroporous adsorption resin for further purification of extracts from Chinese herbal medicines[J].Chinese Journal of New Drugs,2015,24(7):745-749.
[8]申桃.丙烯酸树脂及其复合材料的制备与性能研究[D].成都:电子科技大学,2017.SHEN T.Preparation and study on the properties of acrylic resin and acrylic composites[D].Chengdu:University of Electronic Science and Technology of China,2017.
[9]曾文雪,涂瑶生,王金钱,等.GC测定AB-8树脂中有机残留物间二乙烯苯和对二乙烯苯的含量[J].时珍国医国药,2013,24(4):802-803.ZENG W X,TU Y S,WANG J Q,et al.Determination organic residuum of 1,3-divinylbenzene and 1,4-divinylbenzene in macroporous resin by GC[J].Lishizhen Med Mater Med Res,2013,24(4):802-803.
[10]孙悦,王卫,唐素芳.顶空气相色谱法测定盐酸帕罗西汀中残留的有机溶剂及基质效应考察[J].药物分析杂志,2010,30(5):963-967.SUN Y,WANG W,TANG S F.Determination of residual organic solvents in paroxetine hydrochloride by headspace capillary GC and research of matrix-induced effect[J].Chinese Journal of Pharmaceutical Analysis,2010,30(5):963-967.