Evaluation of Two Fully Automated Setups for Mycotoxin Analysis Based on Online Extraction-Liquid Chromatography–Tandem Mass Spectrometry

Abstract

Mycotoxins are secondary metabolites of fungi species widely known for their potentially toxic effects on human health. Considering their frequent presence in crops and their processed food, monitoring them on food-based matrices is now an important topic. Within such a context, the sample preparation step is usually mandatory before the chromatographic analysis, due to the complexity of matrices such as nuts, cereals, beverages, and others. For these reasons, we herein present the evaluation of two greener setups, based on the automation and miniaturization of the sample preparation step for mycotoxin analysis in different beverages. Firstly, we describe an analytical method based on a multidimensional assembly, coupling a lab-made microextraction column (508 µm i.d. × 100 mm) to a UPLC–MS/MS for the analysis of ochratoxin A in beverages. This configuration used a synthesized sorbent phase containing C18-functionalized graphene–silica particles, which exhibited excellent extraction performance, as well as being reusable and cheaper than commercially available extractive phases. Sequentially, a second setup, based on a multidimensional capillary LC coupled to MS/MS, was assessed for the same purpose. In this case, a graphene oxide-based capillary extraction column (254 µm i.d. × 200 mm) was used as the first dimension, while a C18 analytical capillary column performed the mycotoxin separation in beverages. Although this second one has similarities with the first, we focused mainly on the benefits related to the link between a miniaturized/automated sample preparation device with a capillary LC–MS/MS system, which made our analysis greener. Additionally, the chromatographic efficiency could even be enhanced.

Challenges and Future State for Mycotoxin Analysis: A Review From a Regulatory Perspective

“…In the 2000s, automation studies focused on multimycotoxin sample preparation, but there was relatively little improvement in the degree of automation in sample preparation. Most claims of automated sample preparation in research papers consist of partial automation of sample clean up steps and injection into LC-MS machines. , In 2020, the FDA/Center for Food Safety and Applied Nutrition began the evaluation of a Chemspeed XL Swing system as a research tool for investigating automation in mycotoxin analysis: a system capable of online centrifugation, shaking, solid dispensing, liquid handling, sonicating, blending, and sample transport using a traveling robotic arm. Although the system is capable of automating the entire sample preparation process providing greater standardization for laboratory methods, the instrument still requires human supervision and human decision making .…”

Determination of Patulin in Apple Juice and Apple-Derived Products Using a Robotic Sample Preparation System and LC-APCI-MS/MS

“…Varying degrees of laboratory automation have been demonstrated for mycotoxin analyses using LC-MS [ 26 , 27 , 28 , 29 ], although automated sample preparation has not been documented specifically for the analysis of patulin. Advances in automation technologies can facilitate the consolidation of various sample preparation tools onto one platform, potentially substituting laborious manual processes for a patulin analysis with completely automated sample preparation [ 7 , 30 ].…”

Applicability and Limitations of a Capillary-LC Column-Switching System Using Hybrid Graphene-Based Stationary Phases

“…These phases have been successfully applied in environmental, biological, and food analysis [ 28 , 29 ]. For example, extraction columns (also known as pre-concentration columns) packed with SiGO-C18ec particles have been applied with success in studies of pesticides in sugarcane spirits [ 30 ], mycotoxin separation in beverages [ 31 ], and xanthines in coffee beverages [ 32 ]. Examples of their application in a column-switching setup containing SiGO particles in the extraction column are the determination of β-lactams from environmental water samples [ 33 ], pesticides in sugarcane spirits [ 30 ], and resolution of antidepressant and antiepileptic drugs in urine [ 34 ].…”