【摘要】：目的:建立枸櫞酸托法替尼原料及片劑中對(duì)映異構(gòu)體含量的測(cè)定方法。方法:采用正相高效液相色譜法測(cè)定。色譜條件:以手性柱Chiralpak AD-H(250 mm×4.6 mm,5μm)為色譜柱;以正己烷-異丙醇-甲醇(71∶21∶8)-三乙胺(100∶0.2)溶液為流動(dòng)相;檢測(cè)波長(zhǎng):280 nm;流速:0.5 mL·min~(-1);柱溫:30℃;進(jìn)樣量:5μL。結(jié)果:該方法專屬性良好,片劑中輔料無干擾,對(duì)映異構(gòu)體與相鄰峰的分離度均大于2.0;精密度(RSD=0.0%,n=6)和中間精密度(RSD=5.9%,n=12)良好;加樣回收率為91.2%~96.4%(RSD=3.0%,n=9);檢測(cè)限和定量限分別為0.08μg·mL~(-1)和0.16μg·mL~(-1),分別約為供試品溶液濃度的0.02%和0.04%;線性范圍為0.16~8.00μg·mL~(-1)(r=1.000);供試品溶液至少在34 h內(nèi)穩(wěn)定;3批原料樣品中對(duì)映異構(gòu)體含量分別為:0.01%、0.02%、0.04%;3批制劑(片劑)樣品中對(duì)映異構(gòu)體含量分別為:0.01%、0.02%、0.05%。結(jié)論:本法經(jīng)方法學(xué)驗(yàn)證,可用于測(cè)定枸櫞酸托法替尼原料及片劑中對(duì)映異構(gòu)體雜質(zhì)的含量。
[Abstract]:Objective: to establish a method for the determination of enantiomers in torfatinib citrate raw materials and tablets. Methods: the method was determined by normal phase high performance liquid chromatography (HPLC). The chromatographic conditions were as follows: chiral column Chiralpak AD-H (250 mm 脳 4.6 mm, 5 渭 m), n-hexane-isopropanol-methanol (71:21:8)-triethylamine (100 鈮，

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