Sil 20a xr system

The chromatographic analysis of SYQ was performed on a SIL-20A XR system (Shimadzu, Kyoto, Japan). The separation was conducted by a XBridge^®C18 column (4.6 mm × 100 mm, 3.5 μm) at 30 °C and the injection volume was 2 µL. The mobile phase contained 0.4% formic acid water solution (A) and methanol solution (B) at 0.8 mL/min flow rate with the following gradient elutions: 0–4 min, 7–9% B; 4–6 min, 9–21% B; 6–10 min, 21–35% B; 10–12 min, 35–38% B; 12–16 min, 38–46% B; 16–20 min, 46–64% B; 20–21 min, 64–7% B.
An API5500 triple quadrupole linear ion trap tandem mass spectrometer (AB SCIEX, Framingham, MA, USA) equipped with an electrospray ionization (ESI) source was used for detection. The operating parameters were as follows: ion source temperature, 550 °C; nebulizer gas (GS1) flow, 55 L/min; auxiliary gas (GS2) flow, 55 L/min; curtain gas (CUR) flow, 40 L/min; spray voltage (IS), 4500 V in the positive mode and −4500 V in the negative mode. Detection of analytes was performed in multiple-reaction mode (MRM).

The mass spectrometry detection was performed using an API5500 triple quadrupole mass (AB SCIEX, Framingham, MA, USA). The MS was equipped with an electrospray ionization (ESI) source operating in MRM and under both positive and negative ion modes. The MS parameters were set as follows: gas temperature 550 °C; pressures of nebulizer of MS, 5500 V (positive) and −4500 V (negative); GSI flow 65 L/min; CUR flow 30 L/min and all MS data were acquired and analyzed using the Analyst 1.5.2 software (AB SCIEX, Framingham, MA, USA). The cone voltage and collision energy parameter of each compound were individually optimized.
The chromatographic analysis was performed on a Shimadzu SIL-20A XR system (Shimadzu, Kyoto, Japan), consisting of a binary solvent delivery system and an automatic sampler. A Synergi^TM Hydro-RP 100Å column (100 mm × 2.0 mm, 2.5 μm, (Phenomenex, Los Angeles, CA, USA) was used for eluting samples. The mobile phase was composed of water (A) and acetonitrile (B) using a gradient elution of 30%–52% B at 0–4 min, 52%–75% B at 4–8 min, 75%–90% B at 8–11 min, 90%–30% B at 11–15 min, 30% B at 15–17.10 min. The column temperature was 40 °C, the flow rate kept at 0.4 mL/min, and the sample injection volume was 1 μL.

The chromatographic analysis of Ophiopogonis Radix was performed on an SIL-20A XR system (Shimadzu, Kyoto, Japan). The separation was conducted by a Synergi™ Hydro-RP100Å column (2.0 mm × 100 mm, 2.5 μm) at 30 °C and injection volume was 2 μL. The mobile phase contained 0.1% aqueous formic acid (A) and 0.1% aqueous acetonitrile (B) at 0.4 mL/min flow rate with the following gradient elution: 0–5 min, 98% A; 5–6 min, 98–40% A; 6–8 min, 40–20% A; 8–10 min, 20% A; 10–12 min, 20–98% A; 12–15 min, 98% A.
The mass spectrometry detection was performed using an API4500 triple quadrupole mass (AB SCIEX, Framingham, MA, USA) equipped with an electrospray ionization (ESI) source operating under both positive and negative ion modes. The parameters of MS were set as follows: ionization temperature (TEM): 650 °C, spray voltage: 5500 V (positive) and −4500 V (negative); GSI flow rate: 65 L/min; CUR flow rate: 30 L/min.