## 1 Introduction  
Ochratoxin A (OTA), a mycotoxin produced by certain fungal species, especially Aspergillus and Penicillium, is the most toxic member of the ochratoxin family. It is widely found in grapes and their derived products, including grape juice, raisins, and wine [1, 2, 3]. OTA has been shown to exert potential teratogenic, mutagenic, carcinogenic, and immunosuppressive effects in humans and animals [4]. It has also been classified as a possible human carcinogen (group 2B) by the International Agency for Research on Cancer [4]. Although OTA is less toxic than aflatoxin, it serves as a valuable model toxin for scientific research. _Aspergillus carbonarius_ is recognized as the major OTA-producing fungal species in grapes and their derived products [5, 6, 7, 8]. The contamination of grapes with _A. carbonarius_ leads to the production of secondary metabolites such as volatile compounds during or before OTA production. Notably, the synthesis of volatile compounds is associated with mycotoxin production [9, 10]. Thus, detecting the changes in contents and types of volatile compounds in grapes contaminated with _A. carbonarius_ is of great significance for early OTA detection, to ensure the quality and safety of grapes and their derived products. Currently, high-performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) is widely adopted for detecting the content of OTA due to its high sensitivity and reproducibility [11]. However, it is imperative to perform sample extraction before HPLC-FLD analysis due to the complexity of the fresh or contaminated grape matrix. Among the sample extraction and preparation techniques, the QuECherSR (Quick, Easy, Cheap, Effective, Rugged, Safe) method has gained increasing attention regarding the determination of mycotoxin residues in various matrices because it is easy to operate, rugged, and safe; it also has a reduced number of procedural steps and can effectively eliminate interfering compounds from samples [12; 13; 14]. Additionally, the QuECherSR method has the advantages of rapidity, cost-effectiveness, and high efficacy [15]. Thus, the QuECherSR-HPLC-FLD method was used for the detection of OTA in this study. The headspace solid-phase microextraction (HS-SPME) technique is a solvent-free extraction method that combines extraction and preconcentration into a single step [16]. Furthermore, GC-MS is the main technology used to determine flavor or volatile profiles. Recently, HS-SPME coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS) has gained significant popularity for analyzing volatile compounds. HS-SPME-GC-MS is generally used for the determination of very volatile compounds. Moreover, it has been used to determine the off-flavor in wine [17], microbial volatile organic compounds [18], the volatile composition of grapes [19; 20], pesticide residues, and veterinary drug residues in foods [21; 22]. However, the HS-SPME mode cannot effectively extract fewer volatile and highly water-soluble compounds for GC analysis [23]. Dispersive liquid-liquid microextraction (DLLME), a relatively new sample preparation method developed by [PERSON] et al. [24], can overcome the aforementioned limitation. DLLME has been widely employed for analyzing various chemical compounds in different types of matrices due to its advantages of simplicity, rapidity, cost-effectiveness, and environmental benignity [25]. For instance, DLLME coupled with GC-MS has been used for analyzing volatile compounds in food matrices [23; 26]. Thus, DLLME-GC-MS can complement HS-SPME-GC-MS for aroma profiling, providing a more comprehensive analysis of the volatile compounds in grapes. The present study aimed to achieve the following: (i) Develop a QuECherSR-HPLC method for OTA determination in grapes contaminated with _A. carbonarius_ using low-cost graphite powder as the adsorbent.