海博麦布中对甲苯亚磺酸甲酯、对甲苯亚磺酸乙酯、对甲苯亚磺酸异丙酯残留研究

Residual research of methyl p-toluene sulfinate,ethyl p-toluene sulfinate and isopropyl p-toluene sulfinate in hybutimibe

基于“杂质谱”概念,确立科学杂质研究策略,建立超高效液相色谱-三重四级杆质谱(UPLC-MS/MS)测定海博麦布中基因毒性杂质对甲苯亚磺酸甲酯、对甲苯亚磺酸乙酯、对甲苯亚磺酸异丙酯含量的方法。采用Agilent Eclipse Plus C_(18)色谱柱进行分离,以0.01 mol/L甲酸铵溶液为流动相A,甲醇为流动相B,梯度洗脱,质谱检测器,流速为0.4 mL/min。结果显示,对甲苯亚磺酸甲酯、对甲苯亚磺酸乙酯、对甲苯亚磺酸异丙酯的线性范围均为1.30~10.20 ng/mL,相关系数r均大于0.9990,方法检出限浓度均为0.80 ng/mL,定量限浓度均为2.60 ng/mL,样品加标回收率均为93.48%~112.82%。本方法可以快速、简便、灵敏、准确地定量测定海博麦布中对甲苯亚磺酸甲酯、对甲苯亚磺酸乙酯、对甲苯亚磺酸异丙酯杂质含量。

Based on the concept of impurity profile,a scientific research strategy for impurity was established to determine the content of methyl p-toluene sulfinate,ethyl p-toluene sulfinate and isopropyl p-toluene sulfinatein in hybutimibe by ultra performance liquid chromatography-triple quadrupole mass spectrometer.The determination was performed on an agilent eclipse plus C_(18) column with the mobile phase consisting of 0.01 mol/L ammonium formate(phase A)and methanol(phase B)by gradient elution.The detector was mass spectrum.The flow rate was 0.4 mL/min.The results showed that the linear range of three compounds was 1.30-10.20 ng/mL with the correlation coefficients all higher than 0.9990.The limit of detection was 0.80 ng/mL,and the limit of quantification was 2.60 ng/mL.The recoveries were between 93.48%and 112.82%.The method is rapid,simple,sensitive and accurate for the quantitative determination of mthyl ptoluene slfinate,ethyl p-toluene sulfinate and isopropyl p-toluene sulfinate in hybutimibe.