Department of Pharmacy, Henan Provincial People's Hospital, People's Hospital of Zhengzhou University, Zhengzhou, Henan, 450003, China.
Department of Day Surgery, Henan Provincial People's Hospital, People's Hospital of Zhengzhou University, Zhengzhou, Henan, 450003, China.
Anal Biochem. 2024 Aug;691:115556. doi: 10.1016/j.ab.2024.115556. Epub 2024 May 3.
we developed an effective protein precipitation method for determination of levamlodipine in human plasma using LC-MS/MS. Sample extraction was carried out by using liquid-liquid extraction in 96-well plate format. (S)-Amlodipine-d4 was used as internal standard (IS). The chromatographic separation was achieved using Philomen Chiral MX (2) column (3 μm, 2.1 × 100 mm). Mobile phase A was comprised of Acetonitrile (ACN), Mono ethanol amine (MEA) and Iso-Propyl alcohol (IPA) (1000:1:10, v/v/v), Mobile phase B was IPA-ACN (2:1, v/v). The flow rate was 0.4 mL/min. The total run time of each sample was 4.0 min with gradient elution. LC-MS/MS spectra were generated in positive ion mode, and multiple reaction monitoring (MRM) was used to detect the following transitions: m/z 409.20 → 238.15 for levamlodipine and 415.25 → 240.20 for (S)-Amlodipine-d4 (the IS). The method was linear from 50 to 10000 pg/mL（R＝0.9988489）,and the lower limit of quantification (LLOQ) was 50 pg/mL. This method was applied to a bioequivalence study of levamlodipine.
我们开发了一种有效的蛋白质沉淀法，用于 LC-MS/MS 测定人血浆中的左旋氨氯地平。样品提取采用 96 孔板格式的液液萃取法。（S）-氨氯地平-d4 用作内标（IS）。采用 Philomen Chiral MX（2）柱（3μm，2.1×100mm）实现色谱分离。流动相 A 由乙腈（ACN）、单乙醇胺（MEA）和异丙醇（IPA）（1000:1:10，v/v/v）组成，流动相 B 为 IPA-ACN（2:1，v/v）。流速为 0.4mL/min。每个样品的总运行时间为 4.0min，采用梯度洗脱。LC-MS/MS 谱在正离子模式下生成，采用多重反应监测（MRM）检测以下转换：m/z 409.20→238.15 用于左旋氨氯地平，415.25→240.20 用于（S）-氨氯地平-d4（IS）。方法在 50 至 10000pg/mL 范围内呈线性（R＝0.9988489），定量下限（LLOQ）为 50pg/mL。该方法应用于左旋氨氯地平的生物等效性研究。
