北京生物医学工程

高效液相色谱法测定聚乳酸中乳酸单体残留量

Determination of lactic acid monomer residues in polylactideby high performance liquid chromatography

作者：刘曦林红赛崔永平

单位：北京市医疗器械检验所(北京101111)<p></p>

关键词：聚乳酸；乳酸单体；残留量；高效液相色谱

分类号：R318.04

出版年·卷·期（页码）：2017·36·5（513-516）

摘要：

目的通过高效液相色谱法(high performance liquid chromatography，HPLC)测定聚乳酸材料中乳酸单体的残留量，完善此类材料的质量评价方法。方法用三氯甲烷溶解聚乳酸材料样品后，加入等体积磷酸二氢钾水溶液(20mmol/L，pH=2.87)涡旋振荡，静置分层后取上清液，采用C18 Synergi 4u Hydro-RP 80A 色谱柱，进样20μL，以流速0.6mL/min，磷酸二氢钾水溶液为流动相，柱温30℃，紫外检测波长210nm，外标法定量并进行方法学研究，包括液相色谱系统适应性、线性范围、检出限、定量限、回收率。结果本方法中理论塔板数为10660，拖尾因子为1.32，分离度为3.81，重复性相对标准偏差为0.54%(n=5)，乳酸在浓度1.05~105μg/mL范围内与峰面积保持良好的线性关系(r=0.999979)，检出限为0.42μg/mL，定量限为1.05μg/mL，萃取平均回收率为94.76%(n=6)，其相对标准偏差为3.04%。聚乳酸样品中乳酸单体平均残留量为144.17μg/g。结论高效液相色谱法测定聚乳酸中乳酸单体残留量具有良好的线性范围，准确度高，重复性好，萃取回收率较高且操作简单，可用于聚乳酸材料中乳酸单体残留量测定。

Objective To determinate lactic acid monomer residues in polylactide by high performance liquid chromatography(HPLC)，and to perfect evaluation method of this kind of materials. Methods Polylactide was dissolved in trichloromethane，then monopotassium phosphate solution(20mmol/L，pH=2.87) was added. The mixed solution was oscillated and then kept still. Lactic acid monomer residual in the supernatant was determined by high performance liquid chromatography with C18 Synergi 4u Hydro-RP 80A column. The injection volum was 20μL; the flow rate was 0.6mL/min; the mobile phases was monopotassium phosphate solution(20mmol/L，pH=2.87); the column temperature was 30℃; the UV-light detectation wavelength was 210nm. The methodology consisted of system suitability，linearity range，detectation limit，limit of quantitation，recovery rate. Results In this method,the theoretical plate number was 10660; the tailing factor was 1.32; the resolution was 3.81; the relative standard deviation of the repeatability was 0.54%(n=5); the concentration range 1.05—105μg/mL of lactic acid kept good linear relationships with peak area and the coefficient correlations were 0.999979%; the limit of detection was 0.42μg/mL; the limit of quantitation was 1.05μg/mL; the average extraction recovery rate was 94.76%(n=6) with relative standard deviation of 3.04%. The average content of lactic acid monomer residual in the sample was 144.17μg/g. Conclusions This method is simple and has good linear relationship,high precision and repeatability,which can be applied to determinate lactic acid monomer residues in polylactide.

参考文献：

［1］ASTM. F1925-2009 Standard Specification for Semi-Crystalline Poly(lactide)Polymer and Copolymer Resins for Surgical Implants. American Society for Testing and Materials［S］. 2009.

［2］ASTM.F2579-2010 Standard Specification for Amorphous Poly(lactide)Polymer and Poly(lactide-co-glycolide) Resins for Surgical Implants. American Society for Testing and Materials［S］. 2010.

［3］国家食品药品监督管理总局. YY/T 0661-2008.外科植入物用聚(L-乳酸)树脂的标准规范［S］.北京：中国标准出版社，2008.

［4］国家食品药品监督管理总局. YY/T 0510-2009.外科植入物用无定形聚丙交酯树脂和丙交酯-乙交酯共聚树脂［S］.北京：中国标准出版社，2009.

［5］李红梅，王传栋，李俊起，等. 气相色谱法测定聚乳酸中的单体残留［J］. 生物医学工程研究，2009，28(3)：213-214.

Li HM,Wang CD,Li JQ,et al. Determination of residual lactide in PLA by gas chromatography［J］. Journal of Biomedical Engineering Research,2009,28(3):213-214.

［6］张莉，文燕，齐伟明，等. 毛细管气相色谱法测定眼科手术粘弹剂中乳酸含量［J］. 化学分析计量，2014，23(3)：43-45.

Zhang L,Wen Y,Qi WM,et al. Determination of lactic acid in ophthalmologic surgical viscoelastic agents by capillaty gas chromatography［J］. Chemical Analysis and Meterage,2014,23(3):43-45.

［7］苏国岁，何爱民. 气相色谱-质谱法测定卷烟烟气总粒相物中的乳酸［J］.分析试验室，2006，25(1)：46-48.

Su GS,He AM. Dtermination of lactic acid in total particular matter of cigarette gas by GC-MS［J］. Chinese Journal of Analysis Laboratory,2006,25(1):46-48.

［8］张霞，刘志华，杨光宇，等. 固相萃取富集/气相色谱法测定烟草中的9种有机酸［J］. 分析测试学报，2014，33(5)：61-66.

Zhang X,Liu ZH,Yang GY,et al. Determination of organic acids in tabacoo by solid phase extraction and gas chromatography［J］. Journal of Instrumental Analysis，2014,33(5):61-66.

服务与反馈：

【文章下载】【加入收藏】

提示：您还未登录，请登录！点此登录