RP-HPLC法测定注射用盐酸丁卡因含量、含量均匀度及有关物质

目的: 建立反相HPLC法测定注射用盐酸丁卡因含量、含量均匀度及有关物质。 方法: 采用Agela Venusil XBP C₁₈(L)(4.6 mm×250 mm,5 μm)色谱柱,以甲醇-水(含0.4%三乙胺,用稀磷酸调节pH至3.0)(55∶45)为流动相,流速:1.0 mL·min^-1,检测波长:315 nm(含量及含量均匀度测定波长),308 nm(有关物质测定波长);柱温:35 ℃,进样体积:20 μL。 结果: 盐酸丁卡因在0.2064~41.28μg·mL^-1浓度范围内呈良好线性关系(r=0.9999)(315 nm和308 nm);平均回收率(n=9)为101.3%;杂质a在0.0214~2.14 μg·mL^-1范围内呈良好线性关系(r=0.9996)(308 nm);平均回收率(n=9)为101.4%。 结论: 本法简便、准确,重复性好,专属性强,灵敏度高,可用于注射用盐酸丁卡因的含量、含量均匀度测定和有关物质检查。

Objective: To develop an RP-HPLC for the determination of content,content uniformity and its related substances in tetracaine hydrochloride for injection. Methods: An Agela Venusil XBP C₁₈ (L)(4.6 mm×250 mm,5 μm)column was adopted with a mobile phase of methanol-water(55∶45,containing 0.4% triethylamine,adjusted to pH 3.0 with dilute phosphoric acid).The flow rate was 1.0 mL·min^-1;the detection wavelength for content and content uniformity determination of tetracaine hydrochloride was 315 nm,and the wavelength for the related substance determination was 308 nm.The column temperature was 35 ℃,and the volume of injection was 20 μL. Results: A good linear correlation of tetracaine hydrochloride was observed within the range of 0.2064-41.28μg·mL^-1 (r=0.9999) (315 nm and 308 nm).The average recovery was 101.3% with RSD 1.0% (n=9).The calibration curves of impurity a were 0.0214-2.14 μg·mL^-1 (r=0.9996)(308 nm).The average recovery was 101.4% with RSD 0.5%(n=9). Conclusion: The method is simple,accurate and repeatable,with strong selectivity and high sensitivity.It can be applied to the determination of content,content uniformity and its related substances in tetracaine hydrochloride for injection.

1 People's Republic of China Pharmacopoeia clinical medication information Chemical drugs and biological products volume(中华人民共和国药典临床用药须知化学药品和生物制品卷),2010,123
2 ChP(中国药典).2010.Vol Ⅱ(二部):630
3 USP 34-NF 29.2011.4381
4 EP 6.0.2008.2063
5 CAO Lie-zheng(曹烈臻),FAN Qi(范琦),LIU Xue-hui(刘学辉),et al.Ion-pair RP-HPLC simultaneous determination in gradient elution mode of rizatriptan benzoate and its related substances(RP-HPLC离子对梯度洗脱法同时测定苯甲酸利扎曲普坦含量和有关物质).Chin J Pharm Anal(药物分析杂志),2011,31(2):274
6 HUANG Hua(黄华),CHENG Jun(程俊),TIAN Hai(田海).RP-HPLC determination of two constituents in compound gargarisma tetracaini(RP-HPLC同时测定复方盐酸丁卡因含漱液中2种有效成分的含量).Chin J Pharm Anal(药物分析杂志).2006;26(7):967
7 LIU Wen-ying(刘文英).Pharmaceutical analysis(药物分析).5th Ed(第五版).Beijing(北京):People^,s Medical Publishing House(人民卫生出版社),2004.140
8 CHEN Ning(陈宁),ZHOU Wei(周卫),DING Yi-mei(丁逸梅),et al.Determination of related substances in tetracaine hydrochloride by HPLC(盐酸丁卡因的HPLC法测定). Chin J Pharm(中国医药工业),2010,41(6):453