盐酸兰地洛尔原料药中3-[4-(3-硝基苯磺酰氧基)苯基]丙酸的检测方法学研究

为了检测并控制合成盐酸兰地洛尔原料药物的质量,依托高效液相色谱-三重串联四级杆质谱建立了一种测定其中痕量基因毒性杂质3-4-(3-硝基苯磺酰氧基)苯基]丙酸的方法。方法采用多级反应监测模式,检测灵敏度可达到0.50 mg/kg,加标回收率在91.9%~97.8%之间,且精密度的相对标准偏差为3.28%(n=6),均能满足杂质检测的需要。该研究方法操作简单、结果可靠,可实现快速、低成本检测。

Study on detecting method of 3-［4-(3-nitrobenzene sulfonyl oxygen radicals)phenyl］ propionic acid in the landiolol hydrochloride crude drug

To detect and control the content of trace toxic impurity 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid, which isessential material in the synthesis of landiolol hydrochloride drug, a HPLC with tandem mass spectrometry method was developed to determine the 3-［4-(3-nitrobenzene sulfonyl oxygen radicals) phenyl］ propionic acid in the landiolol hydrochloride crude drug. The multiple reaction monitor mode was used to eliminate the matrix effect and increase the sensitivity of the method. The limit of detection of the target analyte was 0.50 mg/kg. The recoveries of spiked samples were between 91.9% and 97.8%. The relative standard diviation value of precision experiment was 3.28%(n=6). The established method was simple, reliable, fast and low cost,which is able to meet the demand of impurities determination in crude drugs.