Development and validation of a supercritical fluid chromatography method for fast analysis of six flavonoids in Citri Reticulatae Pericarpium

Eco-friendly Deep Eutectic Solvents Contribute to Improving the Separation of Isoquinoline Alkaloids in Supercritical Fluid Chromatography

“…As illustrated in our previous study, mobile phase additives could effectively eliminate the silanol effect on the silica-based stationary phases because the modifier not only increased their affinity to the mobile phase by interacting with the analytes but also competed with the analytes for hydrogen bond donor and receptor sites on the stationary phase Figure A–D illustrates the separation of 10 IQAs with methanol, MeOH-2% H 2 O, MeOH-2% H 2 O-0.5% FA, and MeOH-0.5% FA as modifiers, respectively.…”

“…To develop a satisfactory SFC method for analysis of the 10 IQAs, the influencing parameters were optimized by evaluating the peak shapes and resolutions of the IQAs. , The stationary phase has a great impact on the chromatographic behavior of IQAs in SFC analysis. Initially, four analytical columns with different stationary phases, including Agilent Zorbax SB-C 18 column (4.6 mm × 250 mm, 5 μm), Agilent Zorbax RX-SIL column (2.1 mm × 150 mm, 5 μm), Agilent Zorbax Eclipse XDB-C 8 column (4.6 mm × 150 mm, 5 μm), and Thermo Syncronis Amino column (4.6 mm × 150 mm, 5 μm), were investigated to optimize the peak shapes and resolutions of IQAs . It was observed, as shown in Figure , that the RX-SIL column with a fully hydroxylated silica surface provided relatively satisfactory separation and good peak shapes for the IQAs compared to the other reversed-phase columns.…”

“…The intraday precision was acquired by analyzing the same samples six times within the same day, while the interday test was examined in triplicates for three consecutive days. The stability test was performed by replicate injections of the SC sample at 0, 2, 4, 6, 8, 12, and 24 h. The recovery test was used to evaluate the accuracy of the method by spiking the SC sample powders with low, medium, and high concentrations of the mixed standard solution and then extracting and analyzing using the established procedures …”

“…SFC analysis was performed using an Agilent 1260 Infinity SFC Analytical System equipped with a modified 1260 Infinity LC system, an SFC binary pump, an SFC control module, thermostatic column compartments, an autosampler with a 5 μL loop, and a diode array detector (Agilent Technologies, Santa Clara). 27 Chromatographic separation was conducted on an Agilent Zorbax RX-SIL column (2.1 mm × 150 mm, 5 μm). The analysis was carried out with gradient elution using supercritical carbon dioxide (CO 2 ) (A) and 0.25% ChCl-Gly-0.5% FA-2% H 2 O in methanol (B) Method Validation.…”

Identification of lipophilic components in Citri Reticulatae Pericarpium cultivars by supercritical CO2 fluid extraction with ultra‐high‐performance liquid chromatography–Q Exactive Orbitrap tandem mass spectrometry

“…For example, compound 38 exhibited a protonated molecular ion at m/z 343.1168 [M+H] + and diagnostic fragments at m/z 328.0932 ([M+H‐CH 3 ] + ), 313.0701 ([M+H‐2CH 3 ] + ), and 285.0743 ([M+H‐2CH 3 ‐CO] + ). Therefore, compound 38 was confirmed as 6‐demethoxytangeretin [12]. In addition, with similar MS 2 fragmentation patterns to that of 6‐demethoxytangeretin, six other PMFs (compounds 29, 33, 35, 37, 41, and 53) were also identified in the SFE extracts of CRP [13].…”