A rapid and reliable method for the quantitation of hydroxychloroquine in serum using turbulent flow liquid chromatography-tandem mass spectrometry
A rapid and reliable method for the quantitation of hydroxychloroquine in serum using turbulent flow liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.cca.2013.02.018
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发表时间：
2013-06-05
影响因子：
5
通讯作者：
Clarke, William A.
中科院分区：
文献类型：
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作者：
Fuezery, Anna K.;Breaud, Autumn R.;Clarke, William A.
背景：羟氯喹通常用于治疗系统性红斑狼疮和类风湿性关节炎。目前在实验室中测量全血水平，但至少有一项研究表明血清水平可能同样有用。此外，血清样本是临床实验室中的首选基质类型，因为与全血相比，其复杂性降低。这些观察结果表明，血清羟氯喹水平的临床效用需要使用更大的研究和更强大的检测方法进行重新评估。方法：血清经0.33mol/L高氯酸沉淀蛋白后，以羟氯喹及其氘代类似物为内标物，进样至旋风湍流柱净化。在HypersilGold C8柱上用水和甲醇的梯度（各含0.1%甲酸和10 mmol/l甲酸铵）完成分析分离。结果：该方法在15.7 ~ 2000 ng/ml范围内线性关系良好。多个水平的总不精密度为
Background: Hydroxychloroquine is routinely used in managing systemic lupus erythematosus and rheumatoid arthritis. Whole blood levels are currently measured in the laboratory but at least one study suggests that serum levels may be equally useful. Moreover; serum samples are the preferred matrix type in the clinical laboratory as a result of their reduced complexity compared to whole blood. These observations suggest that the clinical utility of serum hydroxychloroquine levels needs to be reevaluated using larger studies and more robust assays. We report a turbulent flow LC-MS/MS method we developed for this purpose.Methods: After protein precipitation from serum with 033 mol/l perchloric acid, hydroxychloroquine and its deuterated analog were injected onto a Cyclone turbulent flow column for sample cleanup. Analytical separation was accomplished on a HypersilGold C8 column with a gradient of water and methanol, each containing 0.1% formic acid and 10 mmol/l ammonium formate. Analytes were ionized and detected by electrospray ionization mass spectrometry with multiple reaction monitoring.Results: Our method was linear from 15.7 to 2000 ng/ml. Total imprecision at multiple levels was