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目的建立反相高效液相色谱法测定有机锡类抗癌化合物二-(2,4-二氟苯甲酰异羟肟酸)二苯基合锡(DPDFT)原料药的含量及有关物质。方法分析柱为Diamonsil C18(250 mm×4.6 mm,5μm);以甲醇-水(20∶80,用磷酸调pH至3.0)为流动相;流速为0.8 m Lmin·1;含量测定检测波长为228 nm,有关物质检测波长为246 nm,柱温为25℃。结果样品中待测组分与有关物质分离良好,平均回收率为99.0%,RSD为0.65%(n=9),回归方程为A=1.65×107C-3 286(r=0.999 9),线性范围为1.7～150μg·mL·1。最低检测限为10 ng。结论本方法操作简便快速,结果准确,专属性强,灵敏度高,可同时用于抗癌化合物DPDCT原料药的含量控制及有关物质检查。
OBJECTIVE To establish a reversed-phase high performance liquid chromatography (RP-HPLC) method for the determination of the content and related substances of the organotin anticancer compound diphenyl tin (DPDFT). Methods The analytical column was Diamonsil C18 (250 mm × 4.6 mm, 5 μm). The mobile phase was methanol-water (20:80, adjusted to pH 3.0 with phosphoric acid) and the flow rate was 0.8 m Lmin · 1. The detection wavelength was 228 nm, the detection wavelength of the relevant substance is 246 nm, and the column temperature is 25 ℃. Results The sample was separated from the related substances with an average recovery of 99.0% and a RSD of 0.65% (n = 9). The regression equation was A = 1.65 × 107C-3 286 (r = 0.999 9) 1.7 ~ 150μg · mL · 1. The minimum detection limit is 10 ng. Conclusion The method is simple, rapid, accurate, specific and sensitive. It can be used for the content control of anticancer compound DPDCT and related substances.