CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Science, Dalian 116023, China.
J Chromatogr A. 2011 Jun 10;1218(23):3669-74. doi: 10.1016/j.chroma.2011.04.020. Epub 2011 Apr 14.
Nanoflow liquid chromatography/mass spectrometry (nano-LC/MS) has attracted increasing interest in virtue of high sensitivity, low sample consumption, and minimal matrix effect. In this work a HPLC-Chip/quadrupole time-of-flight (Q-TOF) MS device with a new ultra-high capacity small molecule chip (UHC-Chip) which features a 500 nL enrichment column and a 150 mm × 75 μm analytical column, was evaluated with a drug mixture covering a wide range of polarities. Excellent chromatographic precision with 0.1-0.5% RSD for retention time and 1.7-9.0% RSD for peak area, low limit of detection, good chip-to-chip reproducibility and linearity were obtained by using this UHC-Chip. Compared with the standard HPLC-Chip with 40 nL trapping column, the UHC-Chip showed higher enrichment capability and hence gave a higher response in signal detection. Additionally, 4-30 times increase in sensitivity was obtained compared with conventional LC/MS, which indicated that UHC-Chip/MS was a valuable tool for the quantitative analysis of low level impurities and degradation products in pharmaceuticals. Moreover, satisfactory results obtained from trace drug analysis of serum samples further proved its practicality and potential for use in drug testing and development.
纳升液相色谱/质谱联用（nano-LC/MS）以其高灵敏度、低样品消耗和最小基质效应而受到越来越多的关注。本工作采用 HPLC 芯片/四极杆飞行时间（Q-TOF）MS 装置，结合具有 500 nL 富集柱和 150 mm×75 μm 分析柱的新型超高容量小分子芯片（UHC-Chip），对涵盖广泛极性范围的药物混合物进行了评估。使用该 UHC-Chip 可获得出色的色谱精密度，保留时间的 RSD 为 0.1-0.5%，峰面积的 RSD 为 1.7-9.0%，检测限低，芯片间重现性和线性良好。与具有 40 nL 捕集柱的标准 HPLC-Chip 相比，UHC-Chip 具有更高的富集能力，因此在信号检测中具有更高的响应。此外，与常规 LC/MS 相比，灵敏度提高了 4-30 倍，表明 UHC-Chip/MS 是定量分析药物中低水平杂质和降解产物的有价值工具。此外，从血清样品中痕量药物分析中获得的满意结果进一步证明了其在药物检测和开发中的实用性和潜力。
