HPLC-DAD法同时测定凝胶膜剂中氨甲环酸和维生素C乙基醚的含量

目的：建立HPLC-DAD法用于同时测定凝胶膜剂中氨甲环酸和维生素C乙基醚的含量。方法：采用Ultimate XB C₁₈ （250 mm×4.6 mm，5 μm）色谱柱，以pH 2.5磷酸盐缓冲液-甲醇（60：40）为流动相；流速为0.9 mL·min^-1；氨甲环酸检测波长为220 nm，维生素C乙基醚检测波长为245 nm；进样量20 μL；柱温30℃。结果：凝胶膜剂中氨甲环酸和维生素C乙基醚质量浓度分别在0.020 1～4.016 8 mg·mL^-1和0.005 0～0.353 4 mg·mL^-1线性范围内与峰面积线性关系良好，平均回收率（n=3）分别为100.8%和95.5%，RSD分别为2.2%和1.4%；两者的日内和日间精密度均值均小于2%；含量测定结果均在95.0%～105.0%。结论：该方法准确、简便，专属性强，重现性好，可作为该制剂的质量控制方法。

Objective: To develop an HPLC coupled with diode array detection (DAD) method for the simultaneous determination of tranexamic acid and 3-O-ethyl ascorbyl ether in compound gel. Methods: The Ultimate XB C₁₈ (250 mm×4.6 mm,5 μm)column was used at 30℃,the mobile phase was consisted of phosphate buffer (pH 2.5)-methanol (60:40) at 0.9 mL·min^-1,the injection volume was 10 μL. The detection wavelengts of tranexamic acid and 3-O-ethyl ascorbyl ether were 220 nm for tranexamic acid and 245 nm for 3-O-ethyl ascorbyl ether,respectively. Results: Above-mentioned 2 compounds were separated well and showed an excellent linear relationship in 0.020 1-4.016 8 mg·mL^-1 and 0.005 0-0.353 4 mg·mL^-1,respectively. The average recovery rates(n=3)of tranexamic acid and 3-O-ethyl ascorbyl ether were 100.8% (RSD=2.2%) and 95.5% (RSD=1.4%),respectively. The RSDs of intra -day and inter-day were less than 2%. The determination results of both were between 95.0%-105.0%. Conclusion: The method is accurate,simple,highly specific and reproducible,which is applicable for the quality control of compound tranexamic acid gel.

[1] SANCHEZ NP,PATHAK MA,SATO S,et al.Melasma:a clinical,light microscopic,ultrastructural,and immunofluorescence study[J].J Am Acad Dermatol,1981,4(6):698
[2] 李孜怡,李怀军,赵晶,等.中医药治疗黄褐斑研究进展[J].辽宁中医药大学学报,2018,20(4):169 LI ZY,LI HJ,ZHAO J,et al.Research progress of traditional Chinese medicine in treating chloasma[J].J Liaoning Univ Tradit Chin Med,2018,20(4):169
[3] 吕永丰,李国成,叶琳.氨甲环酸联合氢醌乳膏治疗黄褐斑的疗效分析[J].临床合理用药杂志,2011,4(18):63 Lü YF,LI GC,YE L.Effect analysis of tranexamic acid combined with hydroquinone cream in the treatment of chloasma[J].Chin J Clin Ration Drug Use,2011,4(18):63
[4] WU S,SHI H,WU H,et al.Treatment of melasma with oral administration of tranexamic acid[J].Aesthet Plast Surg,2012,36(4):964
[5] LEE HC,THN TG,GOH CL.Oral tranexamic acid in the treatment of melasma:a retrospective analysis[J].J Am Acad Dermatol,2016,75(2):385
[6] TAN AWM,SEN P,CHUA SH,et al.Oral tranexamic acid lightens refractory melasma[J].Aust J Dermatol,2017,58(3):105
[7] STEINER D,FEOLA C,BIALESKI N.Study evaluating the efficacy of topical and injected tranexamic acid in treatment of melasma[J].Surg Cosm Dermatol,2009,1(4):174
[8] BANDYOPADHYAY D.Topical treatment of melasma[J].Indian J Dermatol,2009,54(4):303
[9] SHANKAR K,GODSE K,AURANGABADKAR S,et al.Evidence-based treatment for melasma:expert opinion and a review[J].Dermatol Ther (Heidelb),2014,4(2):165
[10] VON HC,ERIKSSON SBS,KALLEN R.Tranexamic acid as an aid to reducing blood transfusion requirements in gastric and duodenal bleeding[J].Br Med J,1987,294(6563):7
[11] 二條贞子.トラネキサム酸による肝斑の治療[J].基礎と臨床,1979,13(9):3129
[12] 北京昂立达技术有限责任公司.维C乙基醚在日化中的应用[J].日用化学品科学,2005,28(8):49 Beijing Onlyda Technology Co.Ltd.Application of vitamin C ethyl ether in daily use[J].Deterg Cosmet,2005,28(8):49
[13] 杜宁,王玉,蔡美明,等.高效液相色谱法测定氨甲环酸注射液的含量和有关物质[J].中国药学杂志,2010,45(2):144 DU N,WANG Y,CAI MM,et al.Determination of tranexamic acid injection and its related substances by RP-HPLC[J].Chin Pharm J,2010,45(2):144
[14] 中华人民共和国药典2015年版.二部[S].2015:1143 ChP 2015.Vol Ⅱ[S].2015:1143