反相高效液相色谱法测定原料药3-氯-3’，4’-二羟基二苯甲酮的含量及有关物质

Study on the determination of 3-chloro-3',4'-dihydroxy diphenylmethanone and its related substances by RP-HPLC

目的：建立反相高效液相色谱（RpHPLC）法测定原料药3-氯3’，4’-二羟基二苯甲酮（HP46）的含量及有关物质。方法：采用Diamonsil C1-（250mm×4．6mm，5μm）色谱柱，以甲醇-乙腈-水（用磷酸调节pH至3．0）（65：5：30）为流动相，流速0．8mL·min，检测波长243nm，柱温25℃，外标法测定HP46含量，自身对照法测定有关物质。结果：有关物质与主药分离良好，主药含量高于99％，HP46在3．0-180mg·L-1范围内线性关系良好（r=0．9999），最低检测限1mg·L-1。结论：建立的高效液相色谱方法灵敏性和专属性好，适用于原料药HP46的质量控制、有关物质检测和稳定性检查。

OBJECTIVE To establish a RP-HPLC method for the determination of 3-chloro-3＇ ,4＇-dihydroxy diphenylmethanone （HP46） and its related substances. METHODS HPLC method was carried on a column of Diamonsil C18 （250 mm×4. 6 mm,5μm） with the mobile phase of methanol acetonitrile-water（adjusted the pH value to 3.0 with phosphoric acid）（65：5：30） at the flow rate of 0. 8 mL.min-1 and the detection wavelength was set at 243 nm. The column temperature was 25℃. HP46 was quantified with external standard method. The related substances were determined by the self-control method. RESULTS Related substances and degraded substances were completely separated from HP46. The content of HP46 was above 99%. The calibration curve of HP46 was linear in range from 3.0 to 180 mg.L-1 （r= 0. 9999）. The minimal detection limit was 1 mg·L-1. CONCLUSION The HPLC method has been developed for quality control, detection of related substances and stability study of HP46 with high sensitivity and specificity.