Ogasawara Minoru, Tsuruta Kyoko, Arao Shinsuke
Iatron Laboratories Inc., Tokyo, Japan.
J Chromatogr A. 2002 Oct 11;973(1-2):151-8. doi: 10.1016/s0021-9673(02)01117-2.
A new flame photometric detector for thin-layer chromatography (TLC) was studied to determine sulfur and phosphorus containing compounds in materials with a high boiling point. The detector was integrated with a flame ionization detector into the Iatroscan TLC-flame ionization detection analyzer. The principle of the detector is based on the photometric detection of flame emission of heteroatom in a hydrogen-air flame. The emission spectra of sulfur and phosphorus were measured using dibenzothiophene (DT) and phosphoric acid as source materials. Interference filters of 394 and 526 nm were chosen for spectral isolation of the sulfur and phosphorus emissions. The effects of variation in air flow-rate and scan speed as related to both sulfur and phosphorus compounds were studied in order to define optimum detection conditions. The best result for the detection of DT as a sulfur compound was obtained under combined hydrogen and air flow-rates of 160 and 500 ml/min, respectively, with a scan speed of 30 s/rod. The response to DT was linear in the range of 0.25-4 microg. On the other hand, the most suitable conditions for detecting phosphatidylcholine (PC) as a phosphorus compound were combined hydrogen and air flow-rates of 160 and 1500 ml/min, respectively, with a scan speed of 40 s/rod. The response to PC was linear in the range of 0.25-16 microg. Application of the instrument with selective detection of sulfur and phosphorus compounds was demonstrated using heavy oils and human serum lipids.
研究了一种用于薄层色谱（TLC）的新型火焰光度检测器，以测定高沸点材料中含硫和含磷化合物。该检测器与火焰离子化检测器集成到Iatroscan TLC - 火焰离子化检测分析仪中。该检测器的原理基于对氢 - 空气火焰中杂原子火焰发射的光度检测。以二苯并噻吩（DT）和磷酸作为源材料测量了硫和磷的发射光谱。选择394和526 nm的干涉滤光片用于硫和磷发射的光谱分离。研究了与硫和磷化合物相关的空气流速和扫描速度变化的影响，以确定最佳检测条件。作为硫化合物检测DT的最佳结果分别在氢气和空气流速为160和500 ml/min、扫描速度为30 s/棒的条件下获得。对DT的响应在0.25 - 4 μg范围内呈线性。另一方面，检测作为磷化合物的磷脂酰胆碱（PC）的最合适条件分别是氢气和空气流速为160和1500 ml/min、扫描速度为40 s/棒。对PC的响应在0.25 - 16 μg范围内呈线性。使用重油和人血清脂质证明了该仪器对硫和磷化合物的选择性检测应用。
