HPLC-MS/MS法测定清洁验证中残留物卡前列素氨丁三醇的含量

Determination of carboprost tromethamine residue in cleaning validation by HPLC-MS/MS

目的建立一种HPLC-MS/MS方法测定清洁验证中卡前列素氨丁三醇的残留量。方法实验中所用色谱柱为Hypersil GOLD C_(18)(100 mm×2.1 mm,3μm)柱;以水(A)-甲醇(B)为流动相,梯度洗脱;柱温:35℃;流速:0.4 mL·min^(-1);进样量:2μL;以电喷雾电离源(electrospray ionization,ESI)为离子源,以多反应监测方式(multiple reaction monitoring,MRM)进行负离子扫描。结果卡前列素氨丁三醇在质量浓度4.316~24.90μg·L^(-1)内与峰面积具有良好的线性关系(r=0.999),回收率为92.8%,RSD为5.6%。结论所建立的HPLC-MS/MS法特异性强、灵敏度高,适用于卡前列素氨丁三醇残留量的测定。

Objective To establish an HPLC-MS/MS method for the determination of carboprost tromethamine residue in cleaning validation.Methods The method was carried out with Hypersil GOLD C_(18)column(100 mm×2.1 mm,3μm).The mobile phase was consisted of water(A)-methanol(B)with gradient elution at a flow rate of 0.4 mL·min^(-1)at 35℃.The injection volume was 2μL.The analyte was detected by negative electrospray ionization(ESI)combined with multiple reaction monitoring(MRM)mode.Results Carboprost tromethamine showed a good linearity in the range of 4.316-24.90μg·L^(-1)(r=0.999).The recovery was 92.8%and the RSD was 5.6%.Conclusion The HPLC-MS/MS method is of high specificity and sensitivity.It can be used for the determination of carboprost tromethamine residue.