Measurement of Whole Blood Sirolimus by an HPLC Assay Using Solid-Phase Extraction and UV Detection
Measurement of Whole Blood Sirolimus by an HPLC Assay Using Solid-Phase Extraction and UV Detection
复制标题
使用固相萃取和 UV 检测通过 HPLC 测定全血西罗莫司
作者：
E. Connor;M. Sakamoto;K. Fujikawa;T. Law;N. Rifai
作者开发了一种 HPLC 测定法，使用相对简单的固相萃取和紫外线检测来测定血液西罗莫司浓度。西罗莫司和内标 32-去甲氧基雷帕霉素的保留时间分别为 8.7 和 9.3 分钟。该测定的线性度高达 200 ng/mL，灵敏度为 2.0 ng/mL，在西罗莫司浓度为 6、10、20 和 30 ng/mL 时，日常重现性分别为 8.8、9.8、6.1 和 6.4%。使用该 HPLC 方法和已建立的 LC/MS/MS 测定进行的患者相关性研究显示，斜率为 0.982，截距为 -0.021 ng/mL，相关系数为 0.99 (n = 37)。在测试的 31 种不同药物中，没有任何药物干扰目标药物的测量，回收率研究得出的总体平均回收率为 101.8%。作者得出的结论是，此处描述的方法适用于血液西罗莫司浓度的治疗监测。
The authors developed an HPLC assay for determining blood sirolimus concentration using a relatively simple solid-phase extraction and UV detection. The retention times of sirolimus and the internal standard, 32-desmethoxyrapamycin, are 8.7 and 9.3 minutes, respectively. The assay possesses linearity up to 200 ng/mL, sensitivity to 2.0 ng/mL, and day-to-day reproducibility of 8.8, 9.8, 6.1, and 6.4% at sirolimus concentrations of 6, 10, 20, and 30 ng/mL, respectively. A patient correlation study using this HPLC method and an established LC/MS/MS assay revealed a slope of 0.982 and intercept of −0.021 ng/mL and a correlation coefficient of 0.99 (n = 37). Of the 31 different drugs tested none interfered with the measurement of the drug of interest, and a recovery study gave an overall mean recovery of 101.8%. The authors conclude that the method described here is suited for the therapeutic monitoring of blood sirolimus concentration.