PubMed · 6038463
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C C Shale. 1967. Progress in high-temperature electrostatic precipitation.. https://doi.org/10.1080/00022470.1967.10468962
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This paper describes a comparison between atmospheric pressure chemical ionization (APCI) and the recently introduced atmospheric pressure photoionization (APPI) interface for the LC-MS determination of idoxifene and its major metabolite, SB245419 (SB19), in human plasma. The results indicate that analyte response in APPI is highly dependent on the solvent composition, especially to water in the mobile phase. Other parameters investigated are the mobile phase flow-rate, the chemical noise, and signal suppression by matrix interferences. APPI appears to be six to eight times more sensitive than APCI for idoxifene and its SB245419 metabolite; the response for the SB245420 metabolite is considerably better than for APCI conditions, but still not sufficient for trace level pharmacokinetic determinations in human plasma. The LOQ for the parent drug and its major metabolite were 10 and 25 ng/ml, respectively, in human plasma. From post-column infusion experiments we conclude that there is little difference in matrix suppression between APCI and APPI. From these studies we suggest APPI may be an additional tool in pharmaceutical LC-MS applications.
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An approach for simultaneous determination of the main type A-trichothecenes by liquid chromatography and atmospheric pressure chemical ionization mass spectrometry is described. Parameters for coupling of LC-MS such as cone voltage, nebulizing temperature and the LC flow-rate, were optimized to provide detection of mycotoxins with maximum sensitivity. Furthermore, the effects of cone voltage and temperature on the fragmentation pattern of the tested toxins were studied. Main type A-trichothecenes such as T-2 Toxin, HT-2 Toxin, acetyl T-2 Toxin, diacetoxyscirpenol, monoacetoxyscirpenol (15-acetoxyscirpenol) and neosolaniol were separated on a reversed-phase narrow bore C18 column, using a linear gradient and a flow-rate of 0.3 ml/min. Mass spectra were obtained in positive ion mode for confirmation and quantitation. The method involves extraction and purification of toxins by using multifunctional Mycosep columns. Deuterated T-2 Toxin was used as an internal standard. A linear working range between 80 and 500 microg/kg in matrix with an acceptable correlation coefficient was observed. The developed method was validated by using a blank oats sample. The detection limit in the matrix was found to be between 50 and 85 microg/kg in selected ion mode for all tested A-trichothecenes. Recovery data were found to be between 77 and 101%. Within run and day-to-day precision were determined as having comparable levels to those found using GC methods. Furthermore, the matrix effect was investigated by comparing the internal standard versus the external standard method in quantification studies. In addition, the developed method was applied for the analysis of naturally contaminated oats, maize, barley and wheat samples.