LC-MS测定罗库溴铵缩合物中环氧物的含量

Determination of Epoxy Compound in Rocuronium Bromide Condensation Compound by LC-MS

关键词:  罗库溴铵  环氧物  液质联用  检测

Key words:  rocuronium bromide  epoxy compound  LC-MS  determination

摘要:

目的 采用液相色谱-四级杆质谱法(LC-MS)建立罗库溴铵缩合物中环氧物的检测方法。 方法 色谱柱为Agilent Eclipes XDB-C₁₈(150 mm×2.1 mm，3 μm)，以甲醇-0.1%甲酸溶液为流动相进行梯度洗脱，流速：0.25 mL min^-1，柱温：30 ℃，SIM离子采集方式，采集离子分子量：347.2，APCI离子源，进样量：5 μL。结果 环氧物的定量限为0.000 3%，检测限为0.000 09%，柱温、流速的微小变化不影响检测结果，定量限浓度平均回收率为98.9%(n=3)。结论 本方法灵敏高，准确度高，可用于罗库溴铵缩合物中环氧物限量检测。

Abstract:

OBJECTIVE To establish a LC-MS method for the determination of epoxy compound in rocuronium bromide condensation compound. METHODS The analysis was carried out on an Agilent Eclipes XDB-C₁₈ column(150 mm×2.1 mm, 3 μm), using a gradient elution of methanol and 0.1% formic acid as the mobile phase at a flow rate of 0.25 mL·min^-1 at 30 ℃, ion source was APCI, acquisition mode was SIM positive ionization, and selected ion was m/z 347.2 ([M+H]⁺). RESULTS The LOQ was 0.000 3%, the LOD was 0.000 09%; there was no influence on sample testing when small changes were made in the chromatographic conditions; the average recovery was 98.9% with RSD of 8.41%(n=3). CONCLUSION The method was sensitive, accurate, and suitable for the limit determination of epoxy compound in rocuronium bromide condensation compound.