Aoc 6000 autosampler

(GC-MS) analysis GC-MS-QP2020 (Shimadzu Corp., Kyoto, Japan) measurements were analyzed as previously described [16 (link),18 (link)], which is a modification of a previous method [19 (link)]. Briefly, samples were added to a 20 mL headspace vial and warmed for 5 min at 60 °C. A solid-phase microextraction (SPME) fiber of 50/30 µm DVB/CAR/PDMS (Sigma-Aldrich, Tokyo, Japan) was inserted into the vial, and the components were extracted for 30 min at 60 °C. The SPME fiber was then inserted into a single quadrupole GC–MS system with a GCMS-QP2020 gas chromatograph and an AOC-6000 autosampler (Shimadzu, Kyoto, Japan). The analysis conditions were as follows: carrier gas, helium (constant pressure 150 kPa); row, DB-Heavy WAX 0.25 mm × 60 m, 0.25 µm (Agilent Technologies, CA, USA); vaporization chamber, split 1 min at 250 °C; temperature program, 50 °C for 4 min, with temperature then being increased by 5 °C/min increments and maintained at 250 °C for 15 min; MS conditions, scan range 30–400 m/z; ionization potential, 70 eV; ion source, 200 °C; and transfer line, 250 °C. Both extraction and injection were performed once. Compounds in the obtained particle spectra were estimated using the main EI-MS library software of the NIST/EPA/NIH Mass Spectral Library with Search Program 2017 (NIST17).

The grape berries were manually destemmed and deseeded and then homogenized to obtain the must. The HS-SPME experimental parameters were adapted from a previous study with minor modifications [20 (link),48 (link)]. Briefly, 5 g of grape berries, 2.5 g of sterile distilled water, and 1.5 g of NaCl were placed in a 20 mL headspace vial, and 10 µL of 4-methyl-2-pentanol solution (1.01 g/L) was added as the internal standard. Volatile compound extraction was performed using an AOC-6000 autosampler (Shimadzu, Basel, Switzerland) and an HS-SPME device coupled with a 50/30 µm DVB/CAR/PDMS fiber (Supelco Inc., Bellefonte, PA, USA) after equilibration at 45 °C for 10 min. Then, the fiber was inserted into the extraction head through a spacer, and the extraction was conducted for 30 min. Lastly, the fiber was immediately inserted into the GC injection port in splitless mode for 10 min to desorb the volatile compounds.

A SHIMADZU GC-2030 gas chromatograph (Shimadzu, Kyoto, Japan) coupled with a GCMS-TQ8040 NX mass spectrometer detector, equipped with a SHIMADZU AOC-6000 Autosampler was used. The GC was equipped with a split/splitless injector (injection system set at 250 °C, using a 3.4 mm splitless deactivated liner with glass wool (SHIMADZU)), operated in the splitless mode. The analytical capillary column was a MEGA-5MS capillary column (30 m × 0.25 mm; i.d. × 0.25 mm film thickness). Injection volume was set at 1 μL. The oven temperature was programmed to be maintained at 50 °C for 1 min, increased to 125 °C at a rate of 25 °C min⁻¹, then increased to 300 °C at a rate of 10 °C min⁻¹ and held at this temperature for 15 min. The carrier gas was He, with a flow rate of 1.69 mL min⁻¹. The detector was operating in electron ionization mode, with electron energy of 70 eV. The temperature of the interface and the ion source were 250 °C and 230 °C, respectively. The total GC run time was 36.50 min. For instrument control and data acquisition and processing, the GCMS solution software (Version 4.50) was used. Confirmation of the determined analytes was based on the criteria of retention time and the ion abundance of 3 selected ions. The multiple reaction monitoring (MRM) mode was used for quantitative analysis. The quantification and qualification ions in the pesticides are listed in Table S1.

All GC-qMS analyses were carried out on a Shimadzu GC2010 and a TQ8050 triple quadrupole mass spectrometer (Shimadzu, Columbia, MD, USA) equipped with an AOC-6000 autosampler. The single quadrupole acquisition mode was exploited on the TQ8050 MS. The SPME fiber was desorbed into the GC inlet at 250 °C for 2 min in splitless mode. Data were acquired by using the GCMS solution software ver. 4.45 (Shimadzu).
The column employed was an SLB-5 ms [(silphenylene polymer, practically equivalent in polarity to poly (5% diphenyl/95% methylsiloxane)], with the following dimensions: 30 m × 0.25 mm ID × 0.25 μm d_f (Supelco, Bellefonte, DE, USA). GC temperature program: 40 °C (hold 1 min) −240 °C at 3 °C/min, then to 350 at 20 °C/min. Helium head pressure (constant linear velocity mode 35 cm/s) was 48 kPa. The MS system was run in full-scan conditions: scan speed 2000 amu/s; mass range 45–400 m/z. Interface and ion source temperatures: 200 and 250 °C.