Gapeev Alexei, Berton Alberto, Fabris Daniele
Department of Chemistry and Biochemistry, University of Maryland, Baltimore County, Baltimore, Maryland, USA.
J Am Soc Mass Spectrom. 2009 Jul;20(7):1334-41. doi: 10.1016/j.jasms.2009.03.007. Epub 2009 Mar 14.
The hypothesis that direct determination of electrospray current would provide a viable method for maintaining spray stability to enable optimal nanospray analysis was tested by building a feedback apparatus capable of reading the current and readjusting the emitter voltage in real time. The apparatus consists of a current-sensing circuit that reads the voltage drop across a resistor located between the high-voltage power supply and the nanospray emitter. A low voltage proportional to the observed current is generated and sent to a data acquisition card. The information is used by a proportional-derivative-integral (PID) algorithm to calculate the magnitude of a low-voltage signal that is used to control the power supply output. Any variation of current across the sensing resistor is thus counteracted by an opposite-direction variation of the high voltage applied to the nanospray emitter. In this way, the apparatus adjusts the emitter voltage to achieve a preset value of current, which it strives to maintain over time in spite of any possible variation of the parameters influencing the spray regime. Preliminary results have shown that the feedback apparatus is capable of establishing and maintaining stable spray for samples that are usually considered challenging in traditional voltage-controlled analysis, such as those consisting of nucleic acid solutions with high salt loads. For these types of samples, the total ion count recorded in current-controlled mode was significantly more stable than that observed in voltage-controlled mode. At the same time, overall signal intensities and signal-to-noise ratios were also significantly improved. Setting the target nanospray current to a predefined value and letting the apparatus reach the target without operator intervention enabled the acquisition of viable data from solutions containing up to 2.5 M ammonium acetate, which are ordinarily difficult by traditional manual tuning. A deeper understanding of the current-voltage relationships for samples of very different compositions is expected to enable one not only to predict the target current that should be used for a certain analysis, but also to devise algorithms to change such target as a function of predictable variations of sample properties and analytical conditions. This will allow for optimal performance to be maintained during on-line gradient chromatography in which the nature of the sprayed solution may vary very widely during the course of the analysis.
通过构建一种能够读取电流并实时重新调整发射器电压的反馈装置,对直接测定电喷雾电流将提供一种维持喷雾稳定性以实现最佳纳米喷雾分析的可行方法这一假设进行了测试。该装置由一个电流传感电路组成,该电路读取位于高压电源和纳米喷雾发射器之间的电阻器两端的电压降。产生一个与观察到的电流成比例的低电压,并将其发送到数据采集卡。比例-微分-积分(PID)算法使用该信息来计算用于控制电源输出的低电压信号的幅度。因此,传感电阻器上电流的任何变化都会被施加到纳米喷雾发射器上的高压的相反方向变化所抵消。通过这种方式,该装置调整发射器电压以达到预设的电流值,尽管影响喷雾状态的参数可能有任何变化,它仍努力随时间维持该值。初步结果表明,对于在传统电压控制分析中通常被认为具有挑战性的样品,例如那些由高盐负载的核酸溶液组成的样品,反馈装置能够建立并维持稳定的喷雾。对于这些类型的样品,在电流控制模式下记录的总离子计数比在电压控制模式下观察到的要稳定得多。同时,整体信号强度和信噪比也有显著提高。将目标纳米喷雾电流设置为预定义值并让装置在无需操作员干预的情况下达到目标,使得能够从含有高达2.5 M醋酸铵的溶液中获取可行数据,而传统手动调谐通常很难做到这一点。预计对非常不同组成的样品的电流-电压关系有更深入的理解,不仅能够预测用于特定分析的目标电流,还能够设计算法根据样品性质和分析条件的可预测变化来改变此类目标。这将允许在在线梯度色谱过程中保持最佳性能,在该过程中喷雾溶液的性质在分析过程中可能会有很大变化。