A study of ion suppression effects in electrospray ionization from mobile phase additives and solid‐phase extracts

Mallet, Claude R.; Lu, Zhenhuan; Mazzeo, Jeffrey R.

doi:10.1002/rcm.1276

Cited by 410 publications

(281 citation statements)

References 20 publications

(29 reference statements)

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“…Therefore, it was noted that reagents used to precipitate proteins were not responsible for the matrix effect. On the other hand, when a small portion of solvent (1:1) is used in protein precipitation methods endogenous compounds, including fatty acids, triglycerides, nucleotides and salts will be present in the post-treated sample and could interfere in the ionization of the analyte leading to ion suppression [32]. Furthermore, since CyA is mainly bound to erythrocytes, whole blood is the matrix of choice for drug determination [33], so that more interferences are present in the post-treated sample.…”

Section: Recovery and Matrix Effectmentioning

confidence: 99%

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Guada

Imbuluzqueta

Mendoza

et al. 2013

Journal of Chromatography B

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Cyclosporine A (CyA) is an immunosuppressant cyclic undecapeptide used for the prevention of organ transplant rejection and in the treatment of several autoimmune disorders. An ultra high performance liquid chromatography-tandem mass spectrometry method (UHPLC-MS/MS) to quantify CyA in lipid nanosystems and mouse biological matrices (whole blood, kidneys, lungs, spleen, liver, heart, brain, stomach and intestine) was developed and fully validated.Chromatographic separation was performed on an Acquity UPLC ® BEH C18 column with a gradient elution consisting of methanol and 2 mM ammonium acetate aqueous solution containing 0.1% formic acid at a flow rate of 0.6 mL/min. Amiodarone was used as internal standard (IS). Retention times of IS and CyA were 0.69 min and 1.09 min, respectively. Mass spectrometer operated in electrospray ionization positive mode (ESI+) and multiple reaction monitoring (MRM) transitions were detected, m/z 1220.69→1203.7 for CyA and m/z 646→58 for IS. The extraction method from biological samples consisted of a simple protein precipitation with 10% trichloroacetic acid aqueous solution and acetonitrile and 5 µL of supernatant were directly injected into the UHPLC-MS/MS system. Linearity was observed between 0.001 µg/mL-2.5 µg/mL (r ≥ 0.99) in all matrices. The precision expressed in coefficient of variation (CV) was below 11.44% and accuracy in bias ranged from −12.78% to 7.99% including methanol and biological matrices. Recovery in all cases was above 70.54% and some matrix effect was observed. CyA was found to be stable in post-extraction whole blood and liver homogenate samples exposed for 6 h at room temperature and 72 h at 4 o C. The present method was successfully applied for quality control of lipid nanocarriers as well as in vivo studies in BALB/c mice.

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Section: Recovery and Matrix Effectmentioning

confidence: 99%

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Guada

Imbuluzqueta

Mendoza

et al. 2013

Journal of Chromatography B

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“…The LOD of this approach was 0.01 ng/ml, whereas the LOQ was 0.05 ng/ml. To verify the absence or presence of the well-known matrix effect, [4] which can lead to signal variation and quantitation errors, the reproducibility of the trypsin digestion reaction using 15 milk samples spiked with 5 ng/ml of enterotoxin A was analyzed by LC-CEC-SACI-MS/MS. The peak areas from milk samples spiked with enterotoxin A were then compared with the areas achieved by analyzing trypsin-digested enterotoxin A in water (Table 1).…”

Section: Lc-rp-esi-ms/ms and Lc-rp-saci-ms/msmentioning

confidence: 99%

“…[2,3] The two commonly used atmospheric pressure ionization sources, electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI), can be influenced by the matrix effect. [4] SACI is, however, less affected by matrix signal suppression effects. [3,5] For example, analyzing undiluted red wine and grape matrix to quantitate ocratoxin does not affect the quantitative performance of SACI.…”

Section: Introductionmentioning

confidence: 98%

Surface‐activated chemical ionization and cation exchange chromatography for the analysis of enterotoxin A

et al. 2009

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Surface-activated chemical ionization (SACI) has been widely used in recent years for the analysis of different compounds (e.g. peptides, street drugs, amino acids). The main benefits of this technology are its high sensitivity and its effectiveness under different chromatographic conditions [i.e. ion exchange chromatography and reversed-phase (RP) chromatography]. Here we used SACI in conjunction with quadrupole time-of-flight mass spectrometry to analyze enterotoxin A, which is produced by Staphylococcus aureus, in milk matrix using both RP and ion exchange chromatographies. SACI had increased sensitivity as compared with electrospray ionization. Moreover, the higher quantitation efficiency of this technique, mainly in terms of limit of detection (0.01 ng/ml), limit of quantitation (0.05 ng/ml), linearity range (0.05-50 ng/ml), matrix effect, accuracy (intraday and interday accuracy errors were 9.2% and 10.3%, respectively) and precision (intraday and interday precision errors were 5.3% and 12.8%, respectively), is shown and discussed.

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“…It is important to bear in mind that the specificity advantage given by MS detectors is often not essential in aflatoxin determination, these compounds usually being the main fluorescent molecules in food matrices. Moreover, when using mass spectrometric detection, although the specificity increases (which is good for qualitative confirmation), problems due to matrix effects seemed to affect the robustness of the quantitative determinations more than with fluorescence detection (Mallet, Lu, & Mazzeo, 2004).…”

Section: Aflatoxinsmentioning

confidence: 99%

Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/mass spectrometry

Sforza

Dall’Asta

Marchelli

2005

Mass Spectrometry Reviews

194

103

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Mycotoxins are fungal toxins produced by molds, which occur universally in food and feed derivatives, and are produced under certain environmental conditions in the field before harvest, post‐harvest, during storage, processing, and feeding. Mycotoxin contamination is one of the most relevant and worrisome problem concerning food and feed safety because it can cause a variety of toxic acute and chronic effects in human and animals. In this review we report the use of mass spectrometry in connection with chromatographic techniques for mycotoxin determination by considering separately the most diffuse class of mycotoxins: patulin, aflatoxins, ochratoxin A, zearalenone, trichothecenes, and fumonisins. Although the selectivity of mass spectrometry is unchallenged if compared to common GC and LC detection methods, accuracy, precision, and sensitivity may be extremely variable concerning the different mycotoxins, matrices, and instruments. The sensitivity issue may be a real problem in the case of LC/MS, where the response can be very different for the different ionization techniques (ESI, APCI, APPI). Therefore, when other detection methods (such as fluorescence or UV absorbance) can be used for the quantitative determination, LC/MS appears to be only an outstanding confirmatory technique. In contrast, when the toxins are not volatile and do not bear suitable chromophores or fluorophores, LC/MS appears to be the unique method to perform quantitative and qualitative analyses without requiring any derivatization procedure. The problem of exact quantitative determination in GC/MS and LC/MS methods is particularly important for mycotoxin determination in food, given the high variability of the matrices, and can be solved only by the use of isotopically labeled internal standards or by the use of ionization interfaces able to lower matrix effects and ion suppressions. When the problems linked to inconstant ionization and matrix effects will be solved, only MS detectors will allow to simplify more and more the sample preparation procedures and to avoid clean‐up procedures, making feasible low‐cost, high‐throughput determination of mycotoxins in many different food matrices. © 2005 Wiley Periodicals, Inc.

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A study of ion suppression effects in electrospray ionization from mobile phase additives and solid‐phase extracts

Cited by 410 publications

References 20 publications

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Surface‐activated chemical ionization and cation exchange chromatography for the analysis of enterotoxin A

Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/mass spectrometry

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