气相色谱-质谱联用法测定间尼索地平含量

GC-MS determination of m-nisoldipine

目的:建立气相色谱-质谱联用(GC-MS)技术测定间尼索地平含量的方法。方法:采用 GC-MS 法,选择离子模式(SIM)检测,以尼莫地平为内标,以 DB-1 ms(0.25 mm×30 m,0.25μm)为毛细管柱,高纯氦气为载气,流速为0.8 mL·min^(-1),选择特征离子 m/z 266.0,210.0和 m/z 296.0,254.0分别对间尼索地平和尼莫地平定量。结果:间尼索地平浓度在2.5～30μg·mL^(-1)范围内呈良好的线性关系(r=0.9993,n=5);精密度、重复性好,RSD 分别为1.6%和1.8%;平均回收率为99.1%(RSD=1.3%,n=9),检测限为0.10 ng。结论:该法快速、准确,灵敏度高,可用于间尼索地平的质量控制。

Objective： To establish a GC - MS method for the assay of m - nisoldipine. Methods： A DB - 1 ms col- umn （0.25 mm× 30 m,0.25 μm） was used with the detector operated in the single -ion monitoring mode with e- lectron -impact ionization（ m/z 266.0,210. 0 for m -nisoldipine and m/z 296.0,254.0 for the internal standard, nimodipine）. The carrier gas was helium with flow rate of 0.8 mL·min - 1. Results： The linearity over the concen- tration range 2.5 - 30 μg · mL- 1 （ r = 0. 9993, n = 5 ） was obtained. The relative standard deviations of the precision and the reproducibility for the proposed method were 1.6% and 1.8%, respectively. The average recovery was 99. 1% （RSD = 1.3% ,n =9） and the detection limit was 0. 10 ng. Conclusion：The method is rapid,accurate,and sensitive and can be used for the quality control of m - nisoldipine.