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《天津医科大学学报》[ISSN:1006-8147/CN:12-1259/R]

卷:

24卷

期数:

2018年01期

页码:

73-77

栏目:

技术与方法

出版日期:

2018-01-20

文章信息/Info

Title:

Quality control of sitagliptin phosphate tablets

文章编号:

1006-8147(2018)01-0073-05

作者:

张金芬; 周禹宏; 李继彬; 邢正英; 房志仲

(天津医科大学药学院, 天津市临床药物关键技术重点实验室,天津 300070)

Author(s):

ZHANG Jin-fen; ZHOU Yu-hong; LI Ji-bin; XING Zheng-ying; FANG Zhi-zhong

(College of Pharmacy,Tianjin Medical University,Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics(Theranostics),Tianjin 300070,China)

关键词:

磷酸西他列汀; 高效液相色谱法; 溶出度; 质量控制

Keywords:

sitagliptin phosphate' target="_blank" rel="external">">sitagliptin phosphate;  HPLC;  dissolution;  quality control

分类号:

R927.11

DOI:

-

文献标志码:

A

摘要:

目的：建立磷酸西他列汀片的质量控制方法。方法：利用HPLC法测定磷酸西他列汀片的含量，色谱条件为：TIANHE? Kromasil C₁₈色谱柱（200×4.6 mm，5 μm）；流动相为甲醇-0.01 mol/L HClO₄=45-55；检测波长λ=205 nm；流速为0.8 mL/min；柱温为25℃；进样量20 μL；采用浆法进行溶出，分别以水、0.01mol/LHCl、PBS4.5及PBS6.8为溶出介质，体积为1 000 mL，转速50 r/min，溶出时间60 min，按照紫外分光光度法（UV）于205 nm波长下进行测定。采用相似因子法对溶出度进行评价。结果：HPLC测定结果显示，磷酸西他列汀在6.4~96 μg/mL的浓度范围内线性关系良好(r=0.999 8)，平均加样回收率为100.74%，RSD为0.46%；UV测定结果显示，磷酸西他列汀在5~15 μg/mL的浓度范围内线性关系良好（水、0.01 mol/L HCl、PBS4.5及PBS6.8中r分别为0.9991、0.999 3、0.999 7、0.999 9）；自制制剂与参比制剂的累积溶出度在4种溶出介质中的相似因子f₍₂₎分别为64、87、63、59，均大于50。结论：该HPLC测定条件和含量测定方法能够有效地测定样品含量，且简便易行；该溶出度测定方法简便、准确度高，适用于磷酸西他列汀片的溶出度测定。

Abstract:

Objective: To establish an appropriate method to determine contents of sitagliptin phosphate tablet. Methods: Content of sitagliptin phosphate tablet was determined by an HPLC method, in which a TIANHE? Kromasil C₁₈ column(200 mm×4.6 mm，5 μm) was used as stationary phase and a mix of methanol-0.1%HClO₄ was used as mobile phase. The detection wavelength was 205 nm and flow rate was 0.8 mL/min. Column temperature was set at 25℃. The paddle method was used to determine the dissolution, using water,0.01mol/L HCl, PBS4.5 and PBS6.8 as mediums respectively with medium volume of 1000mL and rotation speed was 50 r/min, dissolution time 60 min. UV method was used to determine the accumulative dissolution of sitagliptin phosphate with the wavelength of 205 nm. The dissolution rate was evaluated by similar factor method. Results: According to the test results of HPLC, the concentration detection of sitagliptin phosphate showed a fine linearity between 6.4-96 μg/mL(r=0.999 8). The average recovery of sitagliptin phosphate was 101.74%, and the corresponding RSD value was 0.46%. According to the test results of UV, the linear range of sitagliptin phosphate were 5-15 μg/mL(r=0.999 1 in water, r=0.999 3 in 0.01mol/L HCl, r=0.999 7 in PBS4.5, r=0.999 9 in PBS6.8). The similarity factor f₍₂₎ for the cumulative dissolution of the self-made preparations and the reference preparations in the 4 dissolution mediums were 64,87,63 and 59(>50). Conclusion: The detection method in this study is simple and accuracy, so it is appropriate to be used in the quality control of sitagliptin phosphate.

参考文献/References:

[1]American Diabetes Association. Diagnosis andclassification of diabetes mellitus [J]. Diabetes Care, 2013, 36(Suppl 1): S67
[2]胡洁，安富荣．西格列汀治疗2型糖尿病的临床研究进展[J]．医药导报，2013，32(6)：760
[3]汪会琴,胡如英,武海滨,等. 2型糖尿病报告发病率研究进展[J/OL]. 浙江预防医学, 2016,28(1):37
[4]万科,蒋世茂. 2型糖尿病患者药物治疗的研究进展[J]. 临床合理用药杂志, 2017,10(19):166
[5]王小彦, 王玉丽, 徐为人. 近几年治疗糖尿病热点靶点的研究进展 [J]. 药物评价研究, 2012, 35(1):42
[6]刘永贵,解学星,吴疆,等. 治疗2型糖尿病的新靶点药物研究进展[J]. 现代药物与临床, 2015,30(2):222
[7]许菁，王玉丽，徐为人，等.治疗2型糖尿病的新型药物西他列汀[J].中国药物与临床， 2007，7 (11): 861
[8] Aune T, Norat P, Romundstad L J, et al. Breastfeeding and the maternal risk of type 2 diabetes:A systematic review and dose-response meta-analysis of cohort studies[J]. Nutr Metab Cardiovasc Dis, 2014,24(2):107
[9]张鹏. 磷酸西格列汀在2型糖尿病中的应用研究[J]. 中国现代药物应用, 2017,11(13):105
[10]向群. 西格列汀治疗2型糖尿病的效果观察[J]. 临床合理用药杂志, 2017,10(08):37
[11] Barnett A．DPP-4 inhibitors and their potential role inthe management of type 2 diabetes[J]．J Clin Pract , 2006,60(11):1454
[12] Van C, Dyck K, Yi B, et al. Single dose of MK-0431, an inhibitorof dipeptidyl peptidase-IV, raise active GLP-1 levels without causinghypoglycaemia in healthy subjects[J]. Diabetes, 2005, 54:493
[13] Herman G, Hanefeld M, Wu M, et al. Effect of MK-0431,a dipeptidyl peptidase Ⅳ(DPP Ⅳ) inhibitor, on glycaemic control after 12 weeks in patients with type 2 diabetes[J]. Diabetes 2005;54:541
[14]Nauck M A, Meininger G, Sheng D, et al. Efficacy and safety of thedipeptidyl peptidase-4 inhibitor, sitagliptin, comparedto the sulphonylurea glipizide in patients with type 2diabetes inadequately controlled on metformin alone:a randomised, double-blind, non-inferiority trial[J]. Diabetes Obes Metab , 2007,9(2):194
[15]欧洲药典论坛. Pharmeuropa 26.3[S] . 2014:357
[16]美国药典. United States Pharmacopoeia[S]. 2016:5852
[17]孙旭，汤瑶，闻镍，等. RP-HPLC法测定人血浆中磷酸西他列汀药物含量[J]. 中国药事，2009，23(8):758

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备注/Memo

备注/Memo:

作者简介 张金芬（1991-），女，硕士在读，研究方向：药物制剂与质量控制研究；通信作者：房志仲，E-mail: fangzhizhong@tmu.edu.cn。

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更新日期/Last Update: 2018-01-23