超高效液相色谱-质谱联用定性定量测定硫酸阿托品片

Qualitative and quantitative determination of atropine sulfate tablets by UPLC-MS

目的建立超高效液相色谱-质谱联用(UPLC-MS)法对硫酸阿托品片进行定性检测,并用内标法和外标法测定硫酸阿托品含量。方法采用超高效液相色谱串联四级杆质谱仪,色谱条件:Shim- pack XR-ODSⅡ(2.0 mmx75 mm,2.2 μm)色谱柱,柱温为35℃,以乙腈-0.25%甲酸溶液为流动相梯度洗脱。质谱条件:ESI源,多反应监测( MRM),检测离子对( m/z):硫酸阿托品(290.2±124.2,290.2±93. 1)。以保留时间和定性离子对之间的相对丰度定性,以定量离子对峰面积定量。内标法以氢溴酸东茛菪碱为内标。结果内标法和外标法均在0.104μg/ml^3.114 μg/ml浓度内呈现良好的线性关系(r>0.999)。内标法测定时,平均加样回收率为99. 81%,重复性试验RSD为0.66%;外标法测定时平均加样回收率为96.79%,重复性试验RSD为0.98%。2种方法含量测定结果相似,均能满足检测要求。结论UPLC-MS测定硫酸阿托品的方法简便、快速、准确,可有效控制硫酸阿托品片的质量。

Objective To establish a UPLC-MS method for qualitative detection of atropine sulfate tablets and determine atropine sulfate content by intermal standard method and external standard method. Methods Ultra performance liquid chroma- tography tandem quadrupole mass spectrometer was adopted. LC condition: A Shim-pack XR-ODSI (2.0 mm x 75 mm, 2.2 μm) column was used with acetonitrile and 0.25% formic acid solution as the mobile phase for gradient elution. MS condi- tion: electrospray ionization( ESI),and multiple reaction monitoring ( MRM),monitoring by ion pairs : atropine sulfate (290.2→ 124. 2,290.2→93. 1). The retention time and relative intensities of the detected qualitative ion pairs using for qualitative, integrating the signals of the detected quantitative ion pairs using for quantitative. Scopolamine hydrobromide was selected as internal standard in internal standard method. Results The atropine sulfate had good linearity with correlation coffcient > 0.999 in internal standard method and external standard method, ranging from 0. 104 μg/ml to 3. 114 μg/ml. In intermal standard method, the average recovery rate was 99.81 %. Repeatability test showed that RSD values of content was 0. 66%. In external standard method,the average recovery was 96. 79%. Repeatability test showed that RSD value of content was 0. 98%. The two methods were similar in content determination, which could satisfy the exarmination request. Conclusion This method is simple and rapid with qualitative and quantitative accuracy, which can be used for the quality control of atropine sulfate tablets.