Sil 20a auto injector

Specific rotations were obtained by using a JASCO P-2200 digital polarimeter (l = 5 cm). ECD spectroscopy was recorded using a JASCO J-1500 spectrometer. FAB-MS and HR-FAB-MS were recorded by using a JEOL JMS-SX 102 A mass spectrometer. ¹ H NMR spectroscopy was recorded on JEOL ECS400 (400 MHz) and JNM-ECA 600 (600 MHz) spectrometers. ¹³ C NMR spectroscopy was recorded on a JNM-ECA 600 (150 MHz) spectrometer. 2D-NMR experiments were carried out on a JEOL JNM-ECA 600 (600 MHz) spectrometer.
Normal phase silica gel column chromatography was carried out using Silica gel 60 (Kanto Chemical Co., Inc. 63–210 mesh), and reversed phase silica gel column chromatography was carried out using C₁₈-OPN (Nacalai Tesque Co., Inc. 140 μm). High-performance liquid chromatography (HPLC) was performed using a Shimadzu SPD-M20A UV–vis detector, Shimadzu LC-20AD pump, and Shimadzu SIL-20 A auto-injector. COSMOSIL 5C18-MS-II (Nacalai Tesque Co., Inc. 250 × 4.6 mm i.d., 250 × 10 mm i.d., and 250 × 20 mm i.d.) columns were used for analytical and preparative work.

The photocatalytic selective oxidation of benzoic alcohol was performed as follows. A mixture of benzyl alcohol (200 μL, 1.78 mmol), PCN-22 (10 mg) and TEMPO (3 mg, 0.02 mmol) in CH₃CN was transferred into a 30 mL Pyrex bottle and purged with 30 mL min^–1 O₂ flow for 5 minutes. For controlled experiments, 10 mg of TiO₂, TCPP, PCN-224, as well as a mechanical mixture of TiO₂ (2 mg) and TCPP (8 mg) were used instead of PCN-22 under the same conditions. The suspension was continuously stirred and irradiated by a 300 W Xe lamp with a light filter to cut off light of wavelength <450 nm. Every 5 minutes, the reaction mixture was sampled with a 20 μL pipettor after 1, 5, 10, 20, 30, 40 and 120 minutes respectively. The samples were analyzed with HPLC (Shimadzu HPLC System with LC-20AD pump, SIL-20A Autoinjector and SPD-20A UV-vis Detector). The concentration of benzyl alcohol and benzaldehyde are calibrated by standard samples. The conversion and selectivity after two hours for three successive runs is shown in Table S2.† There was no obvious decrease in activity and selectivity after three successive runs, demonstrating a good recyclability of PCN-22 as a recyclable heterogeneous catalyst.

The AmT was analyzed in an analytical CLAE (Shimadzu), with two LC-20AD pumps, SIL-20A auto-injector, SPD-M20A diode array detector (DAD), CBM-20A controller and CTO-20A oven. The chromatograph was also coupled to a microTOFIII mass spectrometer (Bruker Daltonics) with electrospray ionization source and quadrupole time-of-flight analyzer (Q-TOF). The chromatographic column used was Kinetex C-18 (150 x 2.1 mm, Phenomenex), coupled to a pre-column with the same material. The mobile phase was composed by acetonitrile (B) and deionized water (A), both containing 1% of formic acid (v/v) under a flow rate of 0.3 ml/min and the oven temperature was 50 oC. The gradient method applied was: 0–2 min. 3% B (isocratic), 2–25 min. 3 to 25% B, 25–40 min. 25 to 80% B and 40–43 min. to 80% B (isocratic). Followed by washing and reconditioning the column. The molecular formula of each compound was determined based on the error of up to 5 ppm and mSigma below 30.

An analytical Shimadzu LC-20AT apparatus (Shimadzu Corporation, Tokyo, Japan) was used for chromatographic fingerprints, equipped with a CBM-20A system controller, an LC-20AT pump, a CTO-10ASvp column oven, an SPD-M20A UV-vis detector, an SIL-20A autoinjector, a DGU-20A₅ degasser, and a Shimadzu LC-solution work station. All MS data acquisitions were collected using a Vion IMS quadrupole time of flight (Q-TOF) configuration (Waters, Milford, MA, America) equipped with an electrospray ionization (ESI) source. An Ohaus CP224C electronic balance was manufactured by Ohaus Corporation (Tianjin, China). A DFT-50A portable high-speed disintegrator was purchased from Wenling Linda Machinery Corporation (Zhejiang, China). A DFD-700 double-row, four-hole electrothermal constant temperature water bath was purchased from Taisite Corporation (Tianjin, China). A D2012 table high-speed small centrifuge was produced by Scilogex Corporation (Rocky Hill, CT, America).
The HPLC grade methanol was purchased from Fisher Scientific (Fair Lawn, NJ, America). Purified water was purchased from Hangzhou Wahaha Group Co., Ltd. (Hangzhou, China). Analytical grade methanol was purchased from Fuyu Fine Chemicals Co., Ltd. (Tianjin, China). Our laboratory extracted, separated, and purified the reference standards of siebolside B, isograndidentatin A, and sakuranetin with more than 95% purity [3 (link)].

AA was analyzed using Shimadzu chromatographic system with LC-20AT pump, SIL-20A auto-injector, CBM-20A controller, CTO-20AS oven, and SPD-20A detector. Separation of AA was performed in an Inertsil Amide (GL Sciences) column (5 µm, 4.0 mm × 250 mm). Mobile phase consisted of 0.1% formic acid (solvent A) and ACN (solvent B). Chromatographic conditions were as follows: Elution with 92% solvent B for 15 min for the separation of AA, then post run with 92% to 60% for 1 min and maintained at 60% for 5 min to wash out the matrix compounds, and back to 92% for 2 min and maintained at 92% for 10 min. Flow rate was fixed at 0.8 mL/min, column was maintained at 25 °C, the injection volume was 10 µL, and the UV detector was used at 254 nm.

Mefloquine and verapamil were quantified in feline plasma based on modified HPLC method [16 (link)]. The HPLC system consisted of a Shimadzu LC-20AT delivery unit, DGU-20A3 HT degassing solvent delivery unit, SIL-20A auto injector, SPD-20A UV detector and CTO-20A column oven. Shimadzu LC Solution software version 1.24 (Kyoto, Japan) was used for chromatographic control, data collection and data processing. Chromatographic separation was performed with a Microsorb-MV C18 column (250 mm × 4.6 mm i.d., 5.0 μm; Varian, Mulgrave, VIC, Australia) with a 1.0 mm Optic-guard C18 pre-column (Choice Analytical, Thornleigh, NSW, Australia) under a pressure of 1,900 psi at 25°C. The isocratic mobile phase consisted of a mixture of 25 mM sodium phosphate buffer with 1.0% triethylamine adjusted to pH 2.5 and acetonitrile and methanol (50:25:25, v/v/v) at a flow rate of 1.0 mL/min. The injection volume was 10 μL per sample. The diode array detector was set at a wavelength of 220 nm. The retention times of verapamil and mefloquine were approximately 8.5 and 14.5 minutes, respectively.