气相色谱-质谱法测定卡贝缩宫素注射液中12种亚硝胺

Determination of 12 nitrosamines in Carbetocin injection by gas chromatography-mass spectrometry

建立气相色谱-质谱法检测卡贝缩宫素注射液中12种亚硝胺的方法。以二氯甲烷作为萃取剂,萃取卡贝缩宫素注射液中的12种亚硝胺,萃取液经Thermo TG-WAX MS毛细管柱(30 m×0.25 mm,0.25μm)分离,采用气相色谱-质谱法检测,内标法定量。载气为高纯氦气,进样口温度为260℃,柱流量为1.0 mL/min,进样体积为2.0μL,柱温为40℃,传输线温度为230℃,离子源温度为280℃。12种亚硝胺的质量浓度在20~60 ng/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.99,测定结果的相对标准偏差为0.49%~3.37%(n=6),平均回收率为79.39%~106.4%,检出限为1.000~3.003 ng/mL,定量限为3.000~10.01 ng/mL,溶液在室温放置24 h内稳定。该方法灵敏度高、准确度高、专属性强,可用于多肽类药物的亚硝胺检测。

A method for determining 12 nitrosamines in Carbetocin injection was established by gas chromatography-mass spectrometry.Using dichloromethane as an extractant,12 nitrosamines were extracted from Carbetobin injection.The extraction was separated by thermo TG-WAX MS(30 m×0.25 mm,0.25μm),and detected by mass spectrometry,then quantified by internal standard method.High purity helium as the carrier gas,injection port temperature was 260℃,column flow rate was 1.0 mL/min,injection volume was 2.0μL,column temperature was 40℃,transmission line temperature was 230℃,ion source temperature was 280℃.The linear range of 12 nitrosamines was 20-60 ng/mL,the correlation coefficients were more than 0.99,the relative standard devitions of the reproducibility test were 0.49%-3.37%(n=6),the average recovery were 79.39%-106.4%,and the detection limits were 1.000-3.003 ng/mL,the limits of quantification were 3.000-10.01 ng/mL,and the standard solution was stable at room temperature for 24 h.This method has advantages of high sensitivity,accurate determination results,and strong specificity.It should be applied to the detection of nitrosamines in peptide drugs.