Rapid determination of Labetalol in breast milk by ultra performance liquid chromatography-tandem coupled with mass spectrometry
CHEN Yu1 ZHENG Xin2 CHEN Libo1 CHEN Feng1
1.Yulin Institute for Food and Drug Control, Guangxi Zhuang Autonomous Region, Yulin 537000, China;
2.Department of Pharmacy, Yulin Maternal and Children Health hospital, Guangxi Zhuang Autonomous Region, Yulin 537000,China
Abstract:Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for rapid determination of labetalol in breast milk. Methods The breast milk sample was precipitated by a methanol-acetonitrile mixed solution, and after centrifugation, the supernatant was centrifuged for injection. The column was Thermo Scientific Syncronis C18 (100 mm × 2.1 mm, 1.7 μm), the initial mobile phase was 0.2% formic acid solution-acetonitrile (80∶20, V/V), the flow rate was 0.2 mL/min, utilizing a gradient elution program. The MS/MS detection was performed under AJS ESI+ in MRM mode, quantitatived by external standard method. Results The linear range of Labetalol was 1.042-104.2 ng/mL (r = 0.9988),with the low limit of quantitation of 1.042 ng/mL. Accuracy was 92.0%-104.8%, intra-batch and inter-batch relative standard deviations were both below 15%. The absolute recovery in breast milk was 82.2%-92.4%. Conclusion The method is simple, accurate, specific, and with high sensitivity, which can be used for concentration in breast milk monitoring of labetalol.