Nakao Ryuji, Ito Takehito, Hayashi Kazutaka, Fukumura Toshimitsu, Yamaguchi Masatoshi, Suzuki Kazutoshi
Molecular Imaging Center, National Institute of Radiological Sciences, 4-9-1, Anagawa, Inage-ku, Chiba 263-8555, Japan.
J Pharm Biomed Anal. 2009 Sep 8;50(2):245-51. doi: 10.1016/j.jpba.2009.04.016. Epub 2009 Apr 19.
An ultra-fast, sensitive and versatile radio-liquid chromatographic (LC) procedure was developed and validated for quality control (QC) tests of PET radiopharmaceuticals. For a wide variety of radio-probes, the usual LC conditions were used: (1) column: Waters XBridge RP(18) (50 mm x 3.0 mm ID, 2.5 microm), (2) mobile phase: a mixture of three modifiers (90% CH3CN, ammonium phosphate at pH 2.1 and pH 9.3), and (3) detection: UV absorption and NaI(Tl) scintillation. The introduction of a short column packed with small particles of 2.5 microm allowed excellent separation of target analytes within a very short run time of 1 min; only a 3% decline of radioactivity was observed during QC analysis of (11)C-labelled pharmaceuticals. Combining ammonium-phosphate buffer as the mobile-phase component and low-wavelength UV detection led to an improvement in the applicability and sensitivity. All 34 pharmaceuticals investigated could be successfully applied to determine the specific radioactivity, radiochemical and chemical purity with 10-times better sensitivity than traditional LC. We could analyze different pharmaceuticals in a short period since this system utilized a common column and mobile phase. The proposed procedure fulfils the requirements for routine QC tests in terms of rapidity, sensitivity, simplicity and applicability.
开发并验证了一种超快速、灵敏且通用的放射性液相色谱（LC）方法，用于正电子发射断层显像（PET）放射性药物的质量控制（QC）测试。对于多种放射性探针，采用了常规的LC条件：（1）色谱柱：沃特世XBridge RP(18)（50 mm×3.0 mm内径，2.5微米），（2）流动相：三种改性剂的混合物（90%乙腈、pH值为2.1和9.3的磷酸铵），以及（3）检测：紫外吸收和碘化钠（铊）闪烁检测。引入填充有2.5微米小颗粒的短柱，可在1分钟的极短运行时间内实现目标分析物的出色分离；在对（11）C标记药物的QC分析过程中，仅观察到3%的放射性下降。将磷酸铵缓冲液作为流动相成分与低波长紫外检测相结合，提高了适用性和灵敏度。所研究的所有34种药物均可成功用于测定比活度、放射化学纯度和化学纯度，灵敏度比传统LC高10倍。由于该系统使用了通用的色谱柱和流动相，我们能够在短时间内分析不同的药物。所提出的方法在快速性、灵敏度、简便性和适用性方面满足了常规QC测试的要求。
