Shi Wenyan, Lu Xinqiong, Zhang Jianchao, Yu Quan, Wang Xiaohao
Division of Advanced Manufacturing, Graduate School at Shenzhen, Tsinghua University, Shenzhen, 518055, China.
State Key Laboratory of Precision Measurement Technology and Instruments, Department of Precision Instrument, Tsinghua University, Beijing, 100084, China.
Rapid Commun Mass Spectrom. 2018 Dec 30;32(24):2159-2165. doi: 10.1002/rcm.8293.
Capillary sampling of liquids for direct mass spectrometry (MS) analysis is introduced. The low transfer rate of the solution in the capillary will affect the analytical sensitivity and the response time; hence a pulsed capillary introduction (PCI) method was proposed and characterized.
The experiments were carried out using a miniature quadrupole mass spectrometer, and liquid can be spontaneously drawn into the vacuum chamber for subsequent ionization and detection. A simple up-and-down motor platform was used to control the brief contact of the capillary inlet with the liquid sample and implement pulsed injection. The pulsed sampling parameters were optimized based on the characterization and dynamic study of liquid transfer in capillaries.
Compared with continuous capillary introduction (CCI), PCI can reduce the response time of MS analysis from more than half a minute to a few seconds. In addition, it provides better detection sensitivity as the ion signals of all solution components are enhanced and the acquired limit of detection (LOD) of toluene is about eight times lower than CCI analysis. For each analysis, the consumed sample volume is only a few nanoliters and the absolute consumption of the analyte can reach the femtogram level.
The proposed PCI method is proved to be successful in improving the sampling efficiency when performing direct liquid analysis without increasing the vacuum load. A miniature MS instrument with a proper capillary inlet can possess flexible operation modes to meet different application demands.
介绍了用于直接质谱(MS)分析的液体毛细管采样方法。毛细管中溶液的低传输速率会影响分析灵敏度和响应时间;因此,提出并表征了一种脉冲毛细管进样(PCI)方法。
实验使用微型四极杆质谱仪进行,液体可自发吸入真空室进行后续电离和检测。使用一个简单的上下电机平台来控制毛细管入口与液体样品的短暂接触并实现脉冲进样。基于毛细管中液体传输的表征和动态研究,对脉冲采样参数进行了优化。
与连续毛细管进样(CCI)相比,PCI可将MS分析的响应时间从半分钟以上缩短至几秒。此外,它提供了更好的检测灵敏度,因为所有溶液成分的离子信号都得到了增强,甲苯的检测限(LOD)比CCI分析低约八倍。每次分析消耗的样品体积仅为几纳升,分析物的绝对消耗量可达到飞克水平。
所提出的PCI方法在不增加真空负荷的情况下进行直接液体分析时,成功提高了采样效率。配备适当毛细管入口的微型MS仪器可以具有灵活的操作模式,以满足不同的应用需求。