Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

Abstract

Recebido em 19/1/11; aceito em 21/5/11; publicado na web em 22/7/11 A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g -1 , respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

UHPLC-MS/MS Determination of Ochratoxin A and Fumonisins in Coffee Using QuEChERS Extraction Combined with Mixed-Mode SPE Purification

“…Thus, coffee is a matrix where the expensive immune-affinity purification is still widely used, 1−3 even in combination with a highly selective method as LC-MS/MS. 4 The regulatory limits in the EU for roasted and soluble (instant) coffee are 5 and 10 μg/kg, 5 respectively, and with the high contents of matrix interferences, the so-called multimycotoxin methods (dilute and shoot) cannot fulfill the sensitivity requirements at the current time. 6−12 Multi methods are only likely to occur before even more sensitive mass spectrometers are being marketed.…”

“…Determination of mycotoxins in roasted coffee is a significant analytical challenge due to the high contents of interfering material, as compared to, for example, cereal grains. Thus, coffee is a matrix where the expensive immune-affinity purification is still widely used, − even in combination with a highly selective method as LC-MS/MS …”

Developments in mycotoxin analysis: an update for 2011-2012

“…It was applicable at methanol concentrations up to 60% and acetonitrile concentrations up to 48%, which may have potential advantages such as less dilutions before the IAC clean-up and may also minimise restrictions in the use of organic solvents in general. Bandeira et al (2012) described the development and validation of a method based also on the use of IAC cleanup and LC/ESI-MS/MS using matrix matched calibration, for the analysis of OTA in roasted coffee with an LOQ of 3 µg/kg. Among the different multitoxin procedures, and deliberately excluding those applicable to feed and foodstuffs which are included in other sections of this review (see section 9), it was remarkable to see the development and validation by Warth et al (2012) of a rapid multi-biomarker LC/ESI-MS/MS method for the quantitative measurements of 15 mycotoxins and key metabolites in urine, serving as a good example of the potential of this technique, which is able to detect the toxins at sub-ppb levels (0.17 µg/l for OTA) within a short period of time (18 min) and without any prior clean-up, in exposure assessment studies.…”

Occurrence of Ochratoxin A in Coffee: Threads and Solutions—A Mini-Review

“…The highest level of OTA (12.1 µg/kg) was found in a sample from Germany [61]. Although in countries like Argentina, Brazil, France and Portugal, OTA was also detected in samples exceeding the maximum level established by EU, the number of samples was reduced comparing to sampling [62][63][64][65][66]. Despite of the lack of consensus in literature regarding the percentage of toxin that is transferred into beverage during brewing, it is known that home-processing methods can influence the OTA concentration in coffee brews [67][68][69][70][71].…”