SEC-RI-MALLS联用技术测定甲基纤维素的分子量及分子量分布
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摘要
目的:建立利用分子排阻色谱(SEC)与示差检测器(RI)和多角度激光光散射仪(MALLS)联用技术对甲基纤维素分子量及分子量分布进行测定的方法。方法:采用串接有TSKgelguard PWXL(6 mm×40mm)保护柱的TSKgel GMPWXL凝胶色谱柱(7.8 mm×300 mm,13μm),以0.1 mol·L~(-1)硝酸钠溶液为流动相,流速为0.5 mL·min~(-1),柱温及示差检测温度为34℃,对来自国内外3个厂家的10批甲基纤维素样品进行了分子量及其分布的测定。结果:该方法测定各批次样品的重均分子量、数均分子量及分散度结果的误差均未超过5%,对同批次样品多次测定结果的RSD均未超过1.0%。结论:该方法操作简便,准确度及重复性良好,适用于甲基纤维素的分子量及分子量分布的测定,为甲基纤维素的质量控制提供了依据。
Objective:To establish a method for the determination of molecular weight and molecular weight distribution of methyl cellulose by size-exclusion chromatography(SEC)-differential refractive index(RI)-multi-angle laser light scattering(MALLS). Methods:The molecular weights and molecular weight distributions of ten batches of methyl cellulose samples from three manufacturers were determined by using 0.1 mol·L~(-1) NaNO_3 solution as mobile phase with flow rate of 0.5 mL·min~(-1). The chromatographic column consisted of TSKgelguard column PWXL(6 mm×40 mm)as pre-column and TSKgel GMPWXL column(7.8 mm×300 mm,13 μm)as separation column. The column temperature and the temperature of RI detector were operated at 34 ℃. Results:The errors of the weight average molecular weight,the number average molecular weight and the dispersion degree of each batch were not more than 5%,and the RSD for the results of the same batches was not more than 1%. Conclusion:The method is simple and accurate with good reproducibility. It is suitable for the determination of molecular weight and molecular weight distribution of methyl cellulose,and provides a reference for the quality control of methyl cellulose.
Objective:To establish a method for the determination of molecular weight and molecular weight distribution of methyl cellulose by size-exclusion chromatography(SEC)-differential refractive index(RI)-multi-angle laser light scattering(MALLS). Methods:The molecular weights and molecular weight distributions of ten batches of methyl cellulose samples from three manufacturers were determined by using 0.1 mol·L~(-1) NaNO_3 solution as mobile phase with flow rate of 0.5 mL·min~(-1). The chromatographic column consisted of TSKgelguard column PWXL(6 mm×40 mm)as pre-column and TSKgel GMPWXL column(7.8 mm×300 mm,13 μm)as separation column. The column temperature and the temperature of RI detector were operated at 34 ℃. Results:The errors of the weight average molecular weight,the number average molecular weight and the dispersion degree of each batch were not more than 5%,and the RSD for the results of the same batches was not more than 1%. Conclusion:The method is simple and accurate with good reproducibility. It is suitable for the determination of molecular weight and molecular weight distribution of methyl cellulose,and provides a reference for the quality control of methyl cellulose.
引文
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[16]宋彦会,杜中海,于鹏,等.SEC-MALLS法测定羟乙基淀粉130/0.4重均分子量及分子量分布[J].齐鲁药事,2012,31(3):155SONG YH,DU ZH,YU P,et al.Determination of weight average molecular weight and molecular weight distribution of hydroxyethyl starch 130/0.4 by SEC-MALLS[J].Qilu Pharm Aff,2012,31(3):155
[17]SCHAGERLOEF H,JOHANSSON M,RICHARDSON S,et al.Substituent distribution and clouding behavior of hydroxypropylmethyl cellulose analyzed using enzymatic degradation[J].Biomacromolecules,2006,7(12):3474
[2]中华人民共和国药典2015年版.四部[S].2015:500,517ChP 2015.VolⅣ[S].2015:500,517
[3]USP 41-NF 36.VolⅡ[S].2018:2664,6117
[4]BP 2018.VolⅡ[S].2018:257,1215
[5]JPⅩⅦ[S].2016:1228
[6]MITALI D,BIPLAB B,GUNJAN S,et al.Effect of methyl cellulose on gelation behavior and drug release from poloxamerbased ophthalmic formulations[J].Intern J Biol Macromol,2015,72:706
[7]赵颖,宋新波,张丽娟,等.高效凝胶色谱法测定甘草多糖分子量及其分子量分布[J].天津中医药,2015,32(1):46ZHAO Y,SONG XB,ZHANG LJ,et al.Determination of molecular weight and weight distribution in Licorice Polysaccharide by HPGPC[J].Tianjin J Tradit Chin Med,2015,32(1):46
[8]白颖,李建伟.凝胶色谱法测定高聚物的平均分子量及分子量分布[J].塑料科技,2007,35(4):70BAI Y,LI JW.Determination of the average molecular weight and molecular weight distribution of high polymer through gel chromatography[J].Plast Sci Technol,2007,35(4):70
[9]FAN WW,FAN XD,TIAN W,et al.Differential analysis on precise determination of molecular weight of triblock copolymer using SEC/MALS and MALDI-TOF MS[J].Polym Testing,2014,40:116
[10]LIYF,SHEN HW,LYONS JW,et al.Size-exclusion chromatography of ultrahigh molecular weight methylcellulose ethers and hydroxypropylmethylcelluloseethers for reliable molecular weight distribution characterization[J].Carbohydrate Polym,2016,138:290
[11]李京,范慧红.高效体积排阻色谱与多角激光光散射仪联机测定低分子肝素分子量及分子量分布[J].中国药学杂志,2009,44(2):140LI J,FAN HH.Determination of molecular weight and molecular weight distribution of low molecular weight heparin by high performance size exclusion chromatograghy with multiangle laser light scatter[J].Chin Pharm J,2009,44(2):140
[12]吴扬兰,王远亮,杨力.SEC-RI-MALLS技术在香菇多糖分子量与分子量分布分析方面的应用研究[J].药物分析杂志,2011,31(12):2256WU YL,WANG YL,YANG L.Application of SEC-RI-MALLStechnique on the study of lentinan molecular weight and distribution analysis of molecular weight[J].Chin J Pharm Anal,2011,31(12):2256
[13]刘蕊,马博凯,勾新磊,等.基于凝胶渗透色谱-激光光散射联用技术的聚天冬氨酸分子量测定方法的建立[J].食品安全质量检测学报,2016,7(11):4318LIU R,MA BK,GOU XL,et al.Establishment of determination method for the molecular weight of polyasparticacid by gel permeation chromatography-multi-angle light scattering[J].J Food Saf Quali,2016,7(11):4318
[14]黄志萍,马新刚,蒋根杰,等.激光光散射法测定BAG分子量及其分子量分布[J].固体火箭技术,2004,27(3):233HUANG ZP,MA XG,JIANG GJ,et al.Measurement of BAGmolecular weight and its distribution using laser light scattering method[J].J Solid Rocket Technol,2004,27(3):233
[15]王喜云,王远亮,吴扬兰,等.凝胶渗透色谱-十八角激光散射仪(GPC-MALLS)的应用:浓度、流量、温度对高分子分子量及其分布的影响[J].光散射学报,2007,19(1):49WANG XY,WANG YL,WU YL,et al.Use of gel permeation chromatography/eighteen-angle laser scattering(GPC/MALLS):the effect of concentration、flow speed、temperature for macromolecules molecules weight and distribution[J].J Light Scatter,2007,19(1):49
[16]宋彦会,杜中海,于鹏,等.SEC-MALLS法测定羟乙基淀粉130/0.4重均分子量及分子量分布[J].齐鲁药事,2012,31(3):155SONG YH,DU ZH,YU P,et al.Determination of weight average molecular weight and molecular weight distribution of hydroxyethyl starch 130/0.4 by SEC-MALLS[J].Qilu Pharm Aff,2012,31(3):155
[17]SCHAGERLOEF H,JOHANSSON M,RICHARDSON S,et al.Substituent distribution and clouding behavior of hydroxypropylmethyl cellulose analyzed using enzymatic degradation[J].Biomacromolecules,2006,7(12):3474