GC-MS测定富马酸卢帕他定中痕量杂质偶氮二异丁腈

牛明玉; 胡丽娜; 印嘉佳

doi:10.13748/j.cnki.issn1007-7693.2019.04.009

GC-MS测定富马酸卢帕他定中痕量杂质偶氮二异丁腈

Trace Determination of Azodiisobutyronitrile in Rupatadine Fumarate by GC-MS

摘要

摘要: 目的采用气相色谱-质谱联用法测定富马酸卢帕他定中偶氮二异丁腈（azodiisobutyronitrile，AIBN）杂质的含量。方法采用DB-624毛细管柱（30 m×0.25 mm，1.4 μm），程序升温，初始温度为70℃，以12℃·min^-1升到250℃，以氦气为载气，流速为0.6 mL·min^-1，采用电子轰击电离源（EI），在单离子检测模式（SIM）下选择m/z 69、m/z 54和m/z 41进行检测。结果 AIBN浓度在0.155 2~3.103 μg·mL^-1内与峰面积线性关系良好（r²=0.999 8）；检测限为0.045 μg·mL^-1，定量限为0.15 μg·mL^-1，样品中杂质AIBN测定结果的重复性良好，RSD（n=6）为0.31%；杂质AIBN低、中、高浓度的加样回收率（n=3）分别为103.9%，101.0%，99.4%，RSD（n=3）分别为0.03%，0.11%和0.08%。经检测，3批富马酸卢帕他定供试品中AIBN均未检出。结论本方法操作简便，结果准确，灵敏度高，可用于富马酸卢帕他定中AIBN的检测。

Abstract: OBJECTIVE To establish a GC-MS analytical method for the trace determination of azodiisobutyronitrile (AIBN) in Rupatadine Fumarate. METHODS The analytical column was DB-624(30 m×0.25 mm, 1.4 μm). The column temperature was maintained at 70℃, then was raised to 250℃ at the rate of 12℃·min^-1, and the flow rate was 0.6 mL·min^-1, the conditions of GC-MS were optimized. The detection was achieved in EI, and the selected ions were m/z 69, m/z 54 and m/z 41. RESULTS The calibration curve of AIBN was in a good linearity over the range of 0.155 2-3.103 μg·mL^-1(r²=0.999 8). The limit of detection was 0.045 μg·mL^-1, and the limit of quantification was 0.15 μg·mL^-1. Repetition of AIBN was fine, with RSD(n=6) of 0.31%. The recoveries of low, middle and high adding concentrations of AIBN were 103.9%, 101.0% and 99.4%, respectively, and the RSD(n=3) were 0.03%, 0.11% and 0.08%. AIBN was not detected in 3 batches of samples. CONCLUSION The method has been proved to be simple, rapid and reliable, which is applicable for the quality control of AIBN in Rupatadine Fumarate.

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