高效液相色谱法测定原料药中溴芬酸钠及其杂质A含量

Content Determination of Bromfenac Sodium and Its Impurity A in Crude Drug by HPLC

目的建立测定原料药中溴芬酸钠及其杂质A含量的高效液相色谱法。方法采用Hypersil BDS C18色谱柱(250 mm×4. 6 mm,5μm),以甲醇-0. 4%三乙胺溶液(用磷酸调pH至5. 0)(55∶45)为流动相,流速为1. 0 m L/min,检测波长为266 nm,柱温为30℃;外标法测定溴芬酸钠及其杂质A的含量。结果溴芬酸钠及其杂质A质量浓度分别在0. 2～0. 6 mg/m L和0. 2～0. 6μg/m L范围内与峰面积线性关系良好,线性回归方程分别为Y=4. 658×105 X-1. 328×105,r=0. 999 9(n=7)和Y=2 469 X+2 601,r=0. 999 9(n=5);平均回收率分别为99. 99%和98. 61%,RSD分别为0. 39%(n=7)和1. 10%(n=5)。结论该方法快速、准确、专属性好,可用于检测原料药中溴芬酸钠及其杂质A的含量。

Objective To establish an HPLC method for the content determination of bromfenac sodium and its impurity A. Methods Hypersil BDS C18 column（250 mm ×4.6 mm,5 μm） was adopted,the mobile phase was methanol - 0.4% triethylenedi- amine（adjust pH to 5.0 by phosphoric acid） （55：45）,the flow rate was 1.0 mL/min, the detection wavelength was 266 nm,the column temperature was 30 ℃. The bromfenac sodium and its impurity A were determined by external standard method. Results The bromfenac sodium and its impurity A were linear in the range of 0.2- 0. 6 mg/mL and 0.2-0.6 μg/mL, respectively. The linear regression e- quations were Y=4.658×10^5X-1.328×10^5, r=0.999 9（n=7） and Y=2 469X＋2 601, r=0.999 9（n=5）,respectively. The average recovery rates were 99.99% with RSD of 0. 39% （n =7） and 98.61% with RSD of 1. 10% （n = 5）, respectively. ConclusionThe method is rapid,accurate and specific,which can be used for the content determination of sodium bromide and its impurity A in crude drug.