高效液相色谱法测定伏格列波糖口腔速溶膜中伏格列波糖的含量和有关物质
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摘要
建立测定伏格列波糖口腔速溶膜剂中伏格列波糖含量及其有关物质的高效液相色谱法。采用柱后衍生HPLC荧光检测法,利用亲水C_(18)色谱柱,流动相为0. 045%辛烷磺酸钠的磷酸盐缓冲液—甲醇(94∶6),荧光检测器激发波长为350 nm,发射波长为430 nm,柱温为25℃,流动相与荧光试剂流速相同,进样量为100μL。结果显示,伏格列波糖与各个杂质峰分离较好,在25. 0～50. 0μg/mL范围内,伏格列波糖浓度与峰面积的线性关系良好(R=0. 9999),高、中、低3种浓度的加样回收率为98. 81%～101. 58%,RSD为0. 99%～1. 27%,检测限和定量限分别为2 ng和10 ng。实验表明,所建立的方法准确可靠、专属性强,可用于伏格列波糖口腔速溶膜剂的质量控制。
The paper is going to establish an HPLC for the determination of both contents and related substances of voglibose in voglibose oral fast dissolving films. Post-column derivatization fluorescence method was used in the experiment. The analysis was performed on a C_(18) column with 0. 045% sodium octanesulfonate phosphate buffer solution methanol(94 ∶ 6) as mobile phase. The effluents were detected by fluoescence detector with an excitation wave length of 350 nm,an emission wave length of 430 nm and a column temperature of 25 ℃ . The flow rate of the fluorescent reagents was the same as that of the mobile phase. And the injection volume was 100 μL. The results show that the linear relationship between the voglibose concentration and peak area is good(R = 0. 9999) within the range of 25. 0 ～ 50. 0 μg/m L for voglibose. The average recovery rates are from 98. 81% to 101. 58% for three different levels of voglibose,RSD is from 0. 99% to 1. 27%. The quantitation limit and detection limit is 2 ng and 10 ng,respectively. This method is accurate,specific,and suitable for the quality control of voglibose oral fast dissolving films.
The paper is going to establish an HPLC for the determination of both contents and related substances of voglibose in voglibose oral fast dissolving films. Post-column derivatization fluorescence method was used in the experiment. The analysis was performed on a C_(18) column with 0. 045% sodium octanesulfonate phosphate buffer solution methanol(94 ∶ 6) as mobile phase. The effluents were detected by fluoescence detector with an excitation wave length of 350 nm,an emission wave length of 430 nm and a column temperature of 25 ℃ . The flow rate of the fluorescent reagents was the same as that of the mobile phase. And the injection volume was 100 μL. The results show that the linear relationship between the voglibose concentration and peak area is good(R = 0. 9999) within the range of 25. 0 ～ 50. 0 μg/m L for voglibose. The average recovery rates are from 98. 81% to 101. 58% for three different levels of voglibose,RSD is from 0. 99% to 1. 27%. The quantitation limit and detection limit is 2 ng and 10 ng,respectively. This method is accurate,specific,and suitable for the quality control of voglibose oral fast dissolving films.
引文
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[10]祝传勇，刘宁，李强，等．高效液相色谱法测定伏格列波糖片有关物质[J]．中国新药杂志，2017,26(4):443-449．
[11]张秀玲，左文坚．HPLC法柱后衍生荧光测定伏格列波糖片有关物质及含量[J]．中国药品标准，2004,5(5):41-43．
[12]张建中，李旭洲．高效液相色谱柱后衍生荧光测定伏格列波糖胶囊含量[J]．中国医药指南，2011,9(17):213-214．
[13]靳玉祥，杨超莲，王宁，等．柱后衍生因素对伏格列波糖柱后衍生检测的影响[J]．中国卫生检验杂志，2012,22(7):1528-1531．
[14]陈芳，夏怡然，侯惠民．伏格列波糖口溶膜剂的制备及质量评价[J]．中国医药工业杂志，2013,44(10):989-992．
[15]章向群，吴凌华，陈方军，等．高效液相色谱-质谱法测定伏格列波糖片中伏格列波糖含量[J]．浙江大学学报(医学版)，2014,43(2):141-144．
[16]周和平，陈小勇．伏格列波糖合成路线图解[J]．中国医药工业杂志，2006,37(8):574-576.
[2]员建中．西格列汀和伏格列波糖分别联合实时动态胰岛素泵对新诊断2型糖尿病患者的疗效对比[J]．世界最新医学信息文摘，2018,18(48):140．
[3]陈青，卢敏，籍增洋，等．伏格列波糖对合并糖耐量减低老年冠心病患者早期干预治疗的临床研究[J]．中国临床药理学杂志，2015,31(22):2199-2201．
[4]季明，张征，邹大进．伏格列波糖改善首发低血糖的2型糖尿病和糖耐量异常患者的血糖波动[J]．上海医学，2014,37(9):755-757．
[5]叶龙彬，苗红，宁光，等．伏格列波糖胶囊治疗2型糖尿病的多中心、随机、双盲、平行对照临床试验[J]．上海医学，2013,36(1):18-21．
[6]王欣荣，孙敏，何璧梅，等．HPLC-ELSD测定法在伏格列波糖生产中的运用[J]．中国抗生素杂志，2009,34(12):730-733．
[7]曾洁．RID-HPLC法测定伏格列波糖口腔崩解片中伏格列波糖含量[J]．中国药事，2008,22(12):1093-1094．
[8]陈超，赖雪雯，蒋畅．离子色谱法测定伏格列波糖片的含量[J]．海峡药学，2013,25(9):54-55．
[9]楼永明．柱前衍生化气相色谱法测定伏格列波糖片含量[J]．中国药品标准，2010,11(5):357-360．
[10]祝传勇，刘宁，李强，等．高效液相色谱法测定伏格列波糖片有关物质[J]．中国新药杂志，2017,26(4):443-449．
[11]张秀玲，左文坚．HPLC法柱后衍生荧光测定伏格列波糖片有关物质及含量[J]．中国药品标准，2004,5(5):41-43．
[12]张建中，李旭洲．高效液相色谱柱后衍生荧光测定伏格列波糖胶囊含量[J]．中国医药指南，2011,9(17):213-214．
[13]靳玉祥，杨超莲，王宁，等．柱后衍生因素对伏格列波糖柱后衍生检测的影响[J]．中国卫生检验杂志，2012,22(7):1528-1531．
[14]陈芳，夏怡然，侯惠民．伏格列波糖口溶膜剂的制备及质量评价[J]．中国医药工业杂志，2013,44(10):989-992．
[15]章向群，吴凌华，陈方军，等．高效液相色谱-质谱法测定伏格列波糖片中伏格列波糖含量[J]．浙江大学学报(医学版)，2014,43(2):141-144．
[16]周和平，陈小勇．伏格列波糖合成路线图解[J]．中国医药工业杂志，2006,37(8):574-576.