Novel compounds
A complex and composition technology, applied in the field of preparing the composition of the present invention, can solve the problems of expensive manufacture and packaging of biphasic compositions, difficulty in preparing low-moisture oral care compositions, etc.
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Embodiment 1
[0117] Embodiment 1: the synthesis of stannous ascorbyl phosphate and tin ascorbyl phosphate
[0118] Stannous ascorbyl phosphate sample preparation: Dissolve 3.220g sodium ascorbyl phosphate in 100mL water, then add 1.567g SnF 2 . The mixture was stirred until complete dissolution and heated at 60 °C for one hour. The solution was directly analyzed by 13C-NMR and diluted to 5000ppm, then analyzed by LC-MS
[0119] Table 1. Materials details for the synthesis of stannous ascorbyl phosphate
[0120]
[0121] Preparation of tin ascorbyl phosphate sample: 0.644g SnF 2 Dissolve sodium ascorbyl phosphate in 100 mL of water, then add 1.567 g of SnF 4 . The mixture was stirred until complete dissolution and heated at 60 °C for one hour. The solution was directly analyzed by 13C-NMR and diluted to 5000 ppm, then analyzed by LC-MS.
[0122] Table 2. Material details for the synthesis of tin ascorbyl phosphate
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[0124]
Embodiment 2
[0125] Embodiment 2: LC-MS analysis
[0126] Briefly, LC- MS analysis. The capillary LC system is equipped with a capillary binary pump (model G1376A), a DAD detector (G1315C), a micro vacuum degasser (model G4225A), and a column oven (model G1316A). The capillary pump was set in microfluidic mode. LC separation was achieved using an Agilent Zorbax SB-Aq column (Agilent Technologies, Palo Alto, CA, USA, part number 871700-914) with 2.1 mm inner diameter x 50 mm dimensions and a 3.5 μm particle size. The mobile phase was methanol:water / 5:95. The flow rate was 70 μL / min, and the injection volume was 1 μL. The AB Sciex tandem mass spectrometer was operated in negative ion mode under the following conditions: Nitrogen (>99.99%) for curtain gas at 10 psi, ion source gases 1 and 2 at 10 psi and 10 psi, respectively. The ESIIonSpray voltage was set to 5.5kV in the ESI interface. The declustering and entry potentials were set to 80V and 5.5V, respectively. The temperature of th...
Embodiment 3
[0127] Embodiment 3: NMR experiment
[0128] Performed on a Bruker Avance spectrometer (Bruker-Biospin, Billerica, MA, US) with a 5mm CryoProdigy platform 13 C NMR studies, 1 The operating frequency of H is 500.0MHz, 13 C operates at 125.7 MHz in water at 25 °C. use 1 The H decoupling sequence ("zgig" from the Bruker pulse library) acquires all 13 C NMR spectrum.
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