HPLC-APCI

Tateo, F. and Bonomi, M., Fast determination of Sudan I by HPLC/APCI-MS in hot chili, spices, and oven-baked foods, J. Agric. Food Chem., 52, 655, 2004. 

HPLC-APCI-MS data are found to be most useful when the chemical identity of additives in a polymer is already known (verification) otherwise tandem MS... 

Only the particle-beam interface produces El spectra for direct comparisons with computerized library spectra of fragmentation patterns. The other systems enable the relative molecular mass (RMM) of analytes up to 105 and above to be established. An example of an HPLC-APCI separation and identification of some benzodiazepine tranquillizers is shown in Figure 4.39. The most appropriate choice of LC-MS interface for a particular... 

HPLC-APCI separation of a mixture of five benzodiazepines using CH3CN/CH30H/H20 (40/25/35) (wt/vol) as the eluate, with a flow rate of 1.2 ml mim1... 

Immunoaffinity procedures have also been developed to selectively extract corticosteroids from different sample matrices. Thus, Seymour et al. demonstrated the higher efficiency of the immunoaffinity methods compared with the conventional extraction procedures using organic solvents [177]. Immunosorbents have also been used for online procedures followed by HLPC-UV [178, 179], HPLC-APCI-MS [179,180], GC-MS [176,181], or capillary electrophoresis [182]. Poly(hydroxyethyl methacrylate) (HEMA) was evaluated as a support material for the anti-dexamethasone antibodies used in IAC. The online IAC-HPLC-MS allowed determination of dexamethasone and flumethasone in equine urine with LODs in the range 3-4 ng mL-1 [180]. The cross-reactivity values obtained in the ELISA and the recoveries of an IAC-HPLC procedure are presented in Table 7. Bagnati et al. developed an immunoaffinity extraction... 

API-MS methods have been successfully applied to the quantification of M2D-C3-0-(E0)n-Me, with reliable and reproducible results obtained after online HPLC separation [29,30]. The method was used to quantify recoveries of the surfactant from the surface of plant foliage and from solid substrates under controlled laboratory conditions. Extension of the method to environmental samples has not been investigated. The entire linear dynamic range for HPLC-APCI-MS was not determined, but linearity was observed within the required... 

An example of the standard curve data obtained with HPLC—APCI— MS and HPLC-LSD is presented in Table 2.8.4, for comparison. In addition to the lower sensitivity, the reproducibility and correlation of the HPLC-LSD data was far inferior to that obtained by HPLC—APCI—MS. 

Results obtained for the application of HPLC—APCI—MS to the quantification of M2D—C3—O—(EO ) —CH3 recoveries from Chenopo-dium album plant foliage are shown in Table 2.8.5, as compared with HPLC-LSD analysis [29], The improvements in the sensitivity and reproducibility were obtained with the use of HPLC—APCI—MS as the analytical method and the HPLC—APCI—MS method also enabled detection of the n = 3 M2D-C3-0-(E0) -CH3 molecule. 

Relative response of M2D-C3-0-(E0) -Mea as determined by HPLC-LSD and HPLC-APCI-MS... 

Surfactant solution HPLC-LSD %uptake HPLC-APCI-MS %uptake... 

Fig. 2.8.8. APCI-MS and HPLC-APCI-MS of a PEMS and PEG. (a) APCI-FIA-MS(+) overview spectrum of a commercial blend of PEMS showing the precursor PEGs (starting at m/z 300,... A m/z 44 u) from chemical synthesis (b) Averaged APCI-LC-MS(+) mass spectrum of PEMS (RT 10.0-13.5 min) from the chromatogram shown in (c) (c) APCI-LC-MS(+) chromatogram of a commercial blend of PEMS acquired in total ion current (TIC) mode (d)-(g) selected mass traces of [M + NH4P ions of PEMS (m/z 516, 560, 604 and 648) and PEG homologues (m/z 520, 564, 608 and 652) (h) APCI-LC-MS(+) chromatogram of PEG in TIC mode [41].

The recovery of M2D-C3-0-(E0)n-CH3 after exposure to various solid media has been investigated by API-MS, high performance liquid chromatography light scattering mass detection (HPLC-LSD) and HPLC-APCI-MS methods [10]. Recoveries with extraction immediately following application were determined (surfactant concentration 0.1%, surfactant/solid lOmgg-1) with complete recoveries obtained on all media other than the clays illite and montmorillonite (Table 5.5.2) [10]. 

The percentage recoveries of M2D - C -> - 0 - (E 0 ) -CH3 over time in the presence of sand, soil and the clays kaolinite, halloysite and montmorillonite (0.1%, 10 mg g" -1) as determined by HPLC-APCI-MS methods are shown in Fig. 5.5.2 [10]. Validation of the data was obtained by parallel HPLC—LSD analysis (data not shown). 

Tea (Camellia sinensis) is one of the most frequently consumed beverages in the world and, consequently, an important agricultural product [168], It has been proved many times that tea may reduce cholesterol level, hypertension, and shows antioxidant and anti-microbial effects [169], Because of its importance, a considerable number of analytical methods have been developed for the separation and quantitative determination of the constituents of tea [170,171]. Thus, the application of high-speed counter-current chromatography [172,173], and HPLC-APCI-MS [174] have been reported. 

Fig. 2.60. Simultaneous HPLC-APCI-MS (a) and HPLC-UV (b) chromatograms of the soybean pod extract. Chromatographic conditions see in text. Peak identification 1 = 7,4 -dihydroxyflavone-7-0-/l-D-glucoside 2 = luteolin-7-0-/i-D-glucosidc 3 = apigcmn-7-0-/5-l)-glucoside 4 = 7,4 -dihydroxyflavone 5 = apigcnin-7-0-/]-D-ghicosidc-6"-0-malonate 6 = luteolin 7 = apigenin. Reprinted with permission from S. M. Boue el al. [166].

Chesnov, S. Bigler, L. Hesse, M. Detection and Characterization of Natural Polyamines by HPLC-APCI (ESI) MS. Fur. Mass Spectrom. 2002, 8, 1-16. 

Stanaszek R, Piekoszewski W. 2004. Simultaneous determination of eight underivatized amphetamines in hair by high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (HPLC-APCI-MS). J Anal Toxicol 28 77. 

Peroxide explosives are potent explosives that can be made starting from common and easy to obtain raw materials. The analysis of triacetone triperoxide (TATP) and hexamethylenetriper-oxidediamine (HMTD) was successfully carried out by HPLC-APCI-MS in a powder sample as well as in post-blast extracts originating from a forensic case [134]. After RP separation on a C18 column using a methanohwater (75 25 v/v) mobile phase containing ammonium acetate (2.5mM) at a 0.4mL/min flow rate, detection was carried out in positive ion mode. MS-MS analysis of [TATPh-NH4]+ and [HMTD - H]+ as precursor ions was necessary in order to achieve the required sensitivity in the analysis of postblast extracts (LOD 0.8 and 0.08 ng on column, respectively). 

A study using APCI and PB-MS in both the NI and PI modes coupled to HPLC was used to determine four OPPs. The results demonstrated the higher sensitivity of HPLC-APCI-MS compared with HPLC-PB-MS and the potential of both techniques for confirming the presence of pesticide (51). 

Schieber A, Keller P, Streker P, Klaiber I and Carle R, Detection of isorhamnetin glycosides in extracts of apples (Malus domestic acv. Brettacher ) by HPLC-PDA and HPLC-APCI-MS/MS. Phytochem Anal 13 87-94 (2002). 

Kollroser M, Schober C (2002) Simultaneous determination of seven tricyclic antidepressant drugs in human plasma by direct-injection HPLC-APCI-MS-MS with an ion trap detector. Ther Drug Monit 24 537-544... 

Urine Samples deconjugated with -glucoronidase, purified using two-step solid phase extraction HPLC-APCI- MS/MS 1.2 ng/mL (MEHP) 78 91% Blount et al. 2000b... 

Blount BC, Blount K, Milgtam E et al 2000b. Quantitative detection of phthalate metabolites in human urine HPLC-APCi-MS/MS. Anal Chem 72 4127-4134. 

Mottram, H.R. (1999) The Application of HPLC-APCI MS to the Regiospecific Analysis of Triacylglycerols in Edible Oils and Fats. PhD thesis, Department of Chemistry, University of Bristol, UK. Movia, E. and Remoli, S. (1977) Application of enzymic hydrolysis to determine the genuineness of butter., Bollettino dei Chimici dei Laboratori Provinciali, 3, 187-192. 

The photodegradation of XII was enhanced by humic substances (10mgL-1) or in a natural water sampled in a dam (Villerest, France) (7.2 mg CL-1). Formation of the photoproducts was measured by HPLC-atmospheric pressure chemical ionization-MS (HPLC-APCI-MS) using se-... 

APCI has become a popular ionization source for applications of coupled HPLC-MS. Figure 1.33 shows an example of an application of HPLC-APCI coupling [79]. It shows the analysis obtained from extracts of maize plants. Six compounds are identified by mass spectrometry. These compounds have been identified as glucoconjugated DIMBOA (2,4-dihydroxy-7-methoxy-l,4-benzoxazin-3-one) and similar molecules that differ by the number of methoxy groups in the benzene ring and/or by the N-O methylation of the hydroxamate function. This example clearly shows the influence of the analyte on the type of observed molecular species. Indeed, the presence of an acidic group in the compound from peak 1 allows mainly the detection of deprotonated molecular ions, whereas the compound from peak 4 does not contain an acid group and thus leads only to the formation of adduct ions. 

HPLC-APCI analysis of a mixture of glucoconjugated compounds related to DIMBOA. Spectrum from peak 4 does not display the deprotonated molecular species. The molecular mass (3 87 Da) is deduced from the adducts. The sample is obtained from extracts of maize plants. Reproduced (modified) from Cambier V., Hance T., and de Hoffmann E., Phy-tochem. Anal., 10, 119-126,1999. 

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