Stable Isotope Biochemistry Laboratory, SUERC, Rankine Avenue, Scottish Enterprise Technology Park, East Kilbride, Glasgow G75 0QF, UK.
Rapid Commun Mass Spectrom. 2010 Jun 30;24(12):1755-62. doi: 10.1002/rcm.4572.
The introduction of liquid chromatography coupled with isotope ratio mass spectrometry (LC/IRMS) as an analytical tool for the measurement of isotope ratios in non-volatile analytes has somewhat simplified the analytical cycle from sample collection to analysis mainly due to the avoidance of the extensive sample processing and derivatisation that were necessary for gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). Here we test the performance of coupling strong anion exchange to IRMS using only the second commercially available interface; the Liquiface. The system was modified from installation specification to improve peak resolution in the interface and maintain peak separation from the column to the mass spectrometer. The system performance was assessed by the determination of sensitivity, accuracy and precision attained from carbohydrate separations. The system performed satisfactorily after modifications, resulting in maintenance of peak resolution from column to mass spectrometer. The sensitivity achieved suggested that approximately 150 ng carbon could be analysed with acceptable precision (<0.3 per thousand). Accuracy was maintained in the interface as determined by correlation with offline techniques, resulting in regression coefficient of r(2) = 0.98 and a slope of 0.99. The average precision achieved for the separation of seven monosaccharides was 0.36 per thousand. The integration of a carbonate removal device limited the effect of background carbon perturbations in the mass spectrometer associated with eluent gradients, and the coupling of strong anion-exchange chromatography with IRMS was successfully achieved using the Liquiface.
液相色谱-同位素比质谱联用(LC/IRMS)作为一种分析工具,用于测量非挥发性分析物的同位素比值,它在分析周期上,从样品采集到分析,与气相色谱-燃烧-同位素比质谱联用(GC/C/IRMS)相比,在一定程度上有所简化,主要是因为避免了广泛的样品处理和衍生化。在这里,我们仅使用第二个商业接口(Liquiface)来测试将强阴离子交换与 IRMS 耦合的性能。该系统是根据安装规范进行修改的,以提高接口中的峰分辨率,并保持从柱子到质谱仪的峰分离。通过碳水化合物分离来评估系统的性能,以确定获得的灵敏度、准确性和精密度。修改后系统性能良好,从而保持了从柱子到质谱仪的峰分辨率。灵敏度的测定表明,大约可以分析 150ng 的碳,且具有可接受的精度(<0.3 per thousand)。通过与离线技术的相关性来确定接口中的准确性,从而得到回归系数 r(2) = 0.98 和斜率为 0.99。七种单糖分离的平均精密度为 0.36 per thousand。碳酸盐去除装置的集成限制了与洗脱梯度相关的质谱仪中背景碳干扰的影响,并且成功地实现了强阴离子交换色谱与 IRMS 的耦合。