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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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药用辅料星型乙交酯丙交酯共聚物中葡萄糖含量测定研究

Determination of glucose content in pharmaceutical excipients star poly(lactide-co-glycolide) polymers

分类号:R917
出版年·卷·期(页码):2020,40 (6):982-987
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 建立LC-MS/MS分析方法测定星型乙交酯丙交酯共聚物(Glu-PLGA)中葡萄糖的含量,对比分析自制奥曲肽微球与善龙?奥曲肽微球(Sandostatin? LAR)在绝对分子量、支化度、葡萄糖含量等方面的差异。方法: 采用XBridge@Amide色谱柱(250 mm×4.6 mm,5 μm),以75%乙腈水溶液为流动相,等度洗脱,流速0.4 mL·min-1;柱温35℃;进样量5 μL;采用负离子MRM扫描模式,质谱离子化方式为ESI,监测离子对m/z 179.0/89.1、179.0/71.1、179.0/59.2;应用凝胶渗透色谱三联检测系统测定Glu-PLGA绝对重均分子量和支化度。结果: 方法学试验考察结果表明,所建立的LC-MS/MS方法专属性,精密度,重复性良好,在0.001~0.02 mg·mL-1浓度范围内线性关系良好(r=0.999 7,n=5),检测下限为0.000 2 mg·mL-1、定量下限为0.000 67 mg·mL-1,加标回收率(n=6)为93.6%,RSD为2.5%;对于善龙?奥曲肽微球与自制奥曲肽微球的研究,三联检测器和LC-MS/MS测定结果是微球1、微球2与善龙?奥曲肽微球基本一致。结论: 建立的测定Glu-PLGA中葡萄糖的含量LC-MS/MS分析方法相对方便简单,测定结果准确度和灵敏度高,三联检测器和LC-MS/MS方法可以对Glu-PLGA进行定性定量表征研究,为以后此类Glu-PLGA的研究提供借鉴。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a LC-MS/MS method for determination of glucose content in star poly(lactide-co-glycolide) polymers(Glu-PLGA) and compare to Sandostatin? LAR and self-made microspheres from absolute molecular weight,degree of branching,and glucose content. Methods: Separation was performed on an XBridge@Amide column (250 mm×4.6 mm,5 μm) with 75% acetonitrile-water as the mobile phase at flow rate of 0.4 mL·min-1. The column temperature was 35℃ and the sampling volumn was 5 μL. The samples were detected by using electrospray ion source ESI under negative ion MRM scanning mode. Choosing the characteristic molecular peaks of m/z 179.0/89.1,179.0/71.1,and 179.0/59. The absolute weight average molecular weight and branching degree of Glu-PLGA were determined by gel permeation chromatography with triple detection system. Results: The methodological evaluation showed that this method had good specificity,precision,and repeatability. For Glucose,the linearity range was 0.001-0.02 mg·mL-1(r=0.999 7,n=5),the limits of detection and quantification were 0.000 2 mg·mL-1 and 0.000 67 mg·mL-1. The average recoveries (n=6) were 93.6%,RSD=2.5%;For Sandostatin? LAR and self-made microspheres,the results of microspheres 1,microspheres 2 are basically identical to Sandostatin? LAR by the gel permeation chromatography with triple detection system and LC-MS/MS measurements. Conclusion: The LC-MS/MS analysis method for the determination of glucose content in Glu-PLGA is relatively convenient and simple with high accuracy and sensitivity. The gel permeation chromatography with triple detection system and LC-MS/MS methods can be used for qualitative and quantitative characterization of Glu-PLGA,which can provide reference for the future research of Glu-PLGA.

-----参考文献:---------------------------------------------------------------------------------------

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