离子对RP-HPLC法测定美沙拉嗪栓的含量及有关物质

目的:建立测定美沙拉嗪栓含量及有关物质的方法。方法:采用离子对反相高效液相色谱法。色谱柱为Thermo Hypersil gold,流动相A为磷酸盐缓冲液(p H 7.2)-四丁基氢氧化铵(TBAH)-甲醇-水(250∶50∶100∶600,V/V/V/V),流动相B为磷酸盐缓冲液(p H 7.2)-TBAH-甲醇-水(250∶50∶500∶200,V/V/V/V)(梯度洗脱),流速为1.0 ml/min,检测波长为235 nm,柱温为40℃,进样量为20μl。结果:4-氨基苯酚、2,5-二羟基苯甲酸、美沙拉嗪检测质量浓度分别在0.039⁰.79、0.040.79、0.04⁰.81、36.120.81、36.12⁴8.16μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.998 7、0.999 7、0.999 2);精密度、稳定性、重复性试验的RSD≤1.5%;4-氨基苯酚、2,5-二羟基苯甲酸平均加样回收率分别为102.91%、102.33%,RSD分别为1.5%、1.3%(n=9)。结论:该方法准确、简便、灵敏度高、专属性好,可用于美沙拉嗪栓的质量控制。

Content Determination of 5-aminosalicylic Suppository and Its Related Substances by Ion-pair RP-HPLC

OBJECTIVE：To establish a method for the content determination of 5-aminosalicylic suppository and its related substances. METHODS：Ion-pair RP-HPLC method was adopted. The determination was performed on Thermo Hypersil GOLD column with mobile phase A consisted of phosphate buffer（pH 7.2）-TBAH-methanol-water（250 ∶ 50 ∶ 100 ∶ 600,V/V/V/V）and mobile phase B consisted of phosphate buffer（pH 7.2）-TBAH-methanol-water（250 ∶ 50 ∶ 500 ∶ 200,V/V/V/V）（gradient elution）at the flow rate of 1.0 ml/ min. The detection wavelength was set at 235 nm and column temperature was 40 ℃. The sample size was 20 μl.RESULTS：The liner range were 0.039-0.79 μ g/ml for 4-aminophenol（r=0.998 7）,0.04-0.81 μ g/ml for 2,5-dihydroxybenzoic（r=0.999 7）and 36.12-48.16 μg/ml for 5-aminosalicylic（r=0.999 2）. RSDs of precision,stability and reproducibility tests were lower than 1.5%. Average recovery rates of 4-aminophenol and 2,5-dihydroxybenzoic were 102.91%（RSD=1.5%,n=9） and102.33%（RSD=1.3%,n=9）. CONCLUSIONS：The method is accurate,simple,sensitive and specific,and can be used for the quality control of 5-aminosalicylic suppository.