Soparawalla Santosh, Salazar Gary A, Perry Richard H, Nicholas Mark, Cooks R Graham
Department of Chemistry, Purdue University, West Lafayette, IN 47907, USA.
Rapid Commun Mass Spectrom. 2009 Jan;23(1):131-7. doi: 10.1002/rcm.3853.
Desorption electrospray ionization (DESI) is a droplet-based ionization method that is applied to samples in the ambient environment with little or no sample preparation. Its utility for industrial applications is explored here for the case of pharmaceutical cleaning validation. A non-proximate large-area DESI system was built to examine representative areas of the surfaces of reaction vessels used in active product ingredient (API) manufacturing. A large-area sprayer capable of sampling an area of approximately 2.5 cm(2) was coupled with a transport tube to allow sensitive, representative sampling of APIs from a stainless steel surface 1 m away from the mass spectrometer. The system was used to detect the APIs neostigmine, acebutolol, amiloride, amiodarone, ibuprofen, montelukast, potassium clavulanate, and beta-estradiol, at levels as low as 30-10 ng/cm(2), easily satisfying the general acceptable limits set by the pharmaceutical industry. These levels were achieved from surfaces resembling the equipment used in API manufacturing processes at a rate of 30 s per analysis.
解吸电喷雾电离（DESI）是一种基于液滴的电离方法，可在几乎无需样品制备的环境条件下应用于样品。本文针对药物清洁验证的情况探讨了其在工业应用中的效用。构建了一种非近距离大面积DESI系统，用于检查活性药物成分（API）制造中使用的反应容器表面的代表性区域。一个能够对约2.5平方厘米面积进行采样的大面积喷雾器与一根传输管相连，以便从距质谱仪1米远的不锈钢表面灵敏、代表性地采集API样本。该系统用于检测新斯的明、醋丁洛尔、阿米洛利、胺碘酮、布洛芬、孟鲁司特、克拉维酸钾和β-雌二醇等API，检测水平低至30 - 10纳克/平方厘米，轻松满足制药行业设定的一般可接受限度。这些水平是在类似于API制造过程中使用的设备表面上以每次分析30秒的速度实现的。
