Sammartano Antonino, Migliari Silvia, Serreli Giulio, Scarlattei Maura, Baldari Giorgio, Ruffini Livia
Department of Nuclear Medicine and Molecular Imaging, University Hospital of Parma, Via Gramsci, Italy.
Department of Diagnostic, Medical Physics Unit, University Hospital of Parma, Via Gramsci, Parma, Italy.
Indian J Nucl Med. 2023 Jan-Mar;38(1):1-7. doi: 10.4103/ijnm.ijnm_11_22. Epub 2023 Feb 24.
Ga-68-DOTA-peptides targeting somatostatin receptors have been assessed as a valuable tool in neuroendocrine tumors imaging using positron emission tomography (PET). A new selective and sensitive high-pressure liquid chromatography (HPLC) method was developed for determining chemical and radiochemical purity of Ga-68-DOTATATE (PET) tracer. The identification of peaks was achieved on a symmetry C18 column 3 μm 120Å (3.0 mm × 150 mm spherical particles) using (A) water + 0.1% trifluoroacetic acid (TFA) and (B) acetonitrile + 0.1% TFA, as the mobile phases at a flow rate of 0.600 mL/min and monitored at 220 nm. The run time was 16 min.
The method was validated to fulfill International Conference on Harmonization requirements and EDQM guidelines, and it included specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision.
The calibration curve was linear over the concentration range from 0.5 to 3 μg/ml, with a correlation coefficient (r2) equal to 0.999, average coefficient of variation (CV%) 2%, and average bias% did not deviate more than 5% for all concentrations. The LOD and LOQ for DOTATATE were 0.5 and 0.1 μg/mL, respectively. The method was considered precise, obtaining coefficients of variation between 0.22% and 0.52% for intraday and 0.20% and 0.61% for interday precision. Accuracy of method was confirmed with average bias% that did not deviate more than 5% for all concentrations.
All results were acceptable and this confirmed that the method is suitable for its intended use in routine quality control of Ga-68-DOTATATE to guarantee the high quality of the finished product before release.
靶向生长抑素受体的Ga-68-DOTA肽已被评估为使用正电子发射断层扫描（PET）对神经内分泌肿瘤进行成像的一种有价值的工具。开发了一种新的选择性和灵敏的高压液相色谱（HPLC）方法，用于测定Ga-68-DOTATATE（PET）示踪剂的化学纯度和放射化学纯度。使用（A）水+0.1%三氟乙酸（TFA）和（B）乙腈+0.1%TFA作为流动相，流速为0.600 mL/min，在220 nm处进行监测，在3μm 120Å（3.0 mm×150 mm球形颗粒）的对称C18柱上实现峰的鉴定。运行时间为16分钟。
该方法经验证符合国际协调会议要求和欧洲药品质量管理局（EDQM）指南，包括特异性、线性、检测限（LOD）、定量限（LOQ）、准确性和精密度。
校准曲线在0.5至3μg/ml的浓度范围内呈线性，相关系数（r2）等于0.999，平均变异系数（CV%）为2%，所有浓度下的平均偏差%不超过5%。DOTATATE的LOD和LOQ分别为0.5和0.1μg/mL。该方法被认为是精确的，日内精密度的变异系数在0.22%至0.52%之间，日间精密度的变异系数在0.20%至0.61%之间。该方法的准确性通过平均偏差%得到证实，所有浓度下的平均偏差%不超过5%。
所有结果均可接受，这证实了该方法适用于其在Ga-68-DOTATATE常规质量控制中的预期用途，以确保成品在放行前的高质量。
