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首页> 外文期刊>Bioanalysis >Development and validation of an HILIC-MS/MS method by one-step precipitation for chloroquine in miniature pig plasma
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Development and validation of an HILIC-MS/MS method by one-step precipitation for chloroquine in miniature pig plasma

机译:一步法沉淀微型猪血浆中氯喹的HILIC-MS / MS方法的开发和验证

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Background: Quantification of polar compounds such as chloroquine by revered-phase LC is a challenge because of poor retention and silanol interactions with stationary phase. Strong ion-pairing reagents added to mobile phases to improve reversed-phase retention and improve peak shape can be harmful for MS. Results: This new approach provides a rapid and sensitive method for the detection of chloroquine using hydrophilic interaction LC coupled to MS/MS (HILIC-MS/MS). Ammonium formate and formic acid were added to mobile phase to attain good peak shapes and the salified chloroquine as well retained in an HILIC column. Linearity, intra-and inter-day precision, accuracy, recovery, matrix effect and stability were evaluated during the validation process. Conclusion: The validated method has been successfully used in a PK study in miniature pigs, and paves way for future development.
机译:背景:由于保留性差以及硅烷醇与固定相的相互作用,通过反相液相色谱法对极性化合物(例如氯喹)进行定量分析是一个挑战。添加到流动相中的强离子对试剂可改善反相保留率并改善峰形,这可能对质谱有害。结果:这种新方法提供了一种快速灵敏的方法,该方法使用与MS / MS(HILIC-MS / MS)耦合的亲水相互作用LC检测氯喹。将甲酸铵和甲酸添加到流动相中,以获得良好的峰形,并且成对的氯喹也保留在HILIC色谱柱中。在验证过程中评估了线性,日内和日间精度,准确性,回收率,基质效应和稳定性。结论:验证的方法已成功用于小型猪的PK研究,为未来的发展铺平了道路。

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