Separation and detection method of antifungal agent in expanded polystyrene
A technology of expanded polystyrene, separation methods, applied in the direction of measuring devices, analytical materials, preparation of samples for testing, etc.
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Embodiment 1
[0081] The sample was expanded polystyrene containing 1 % TBZ. Weigh 10 g of the sample, crush it with a freeze pulverizer, dissolve the sample in 200 mL of DMSO, keep the reaction temperature at 20 °C, add 50 mL of DMSO solution containing 1 mL of chlorosulfonic acid, and react for 30 min. After the reaction was completed, 250 mL of distilled water was added to the solution, shaken vigorously in a separatory funnel for 10 min, and the aqueous phase was separated. The aqueous phase solution was poured into a supercritical extraction kettle, and the supercritical CO with a temperature of 110 °C and a pressure of 16 MPa was introduced. 2 , extracted for 20 minutes, filtered to remove the solid, and the filtrate was sulfonated TBZ. LC-MS was used for detection. The chromatographic system of LC-MS was Agilent 1200 liquid chromatograph, and the chromatographic column was Agilent Eclipse Plus C18. The mobile phase was 10 mmol / L ammonium acetate aqueous solution (A) and acetonitril...
Embodiment 2
[0083] The sample was expanded polystyrene containing 2.5 % TBZ. Weigh 10 g of the sample, crush it with a freeze pulverizer, dissolve the sample in 200 mL of DMSO, keep the reaction temperature at 20 °C, add 50 mL of DMSO solution containing 1 mL of chlorosulfonic acid, and react for 40 min. After the reaction was completed, 250 mL of distilled water was added to the solution, shaken vigorously in a separatory funnel for 10 min, and the aqueous phase was separated. The aqueous phase solution was poured into a supercritical extraction kettle, and the supercritical CO with a temperature of 110 °C and a pressure of 16 MPa was introduced. 2 , extracted for 20 min, filtered to remove the solid, and the filtrate was sulfonated TBZ. Using LC-MS detection, the detection conditions are the same as in Example 1, the retention time of sulfonated TBZ is 7.2 min, and the M-1 peak is 279. Using dibutyl phthalate as an internal standard, the content of TBZ in the sample was determined to ...
Embodiment 3
[0085] The sample was expanded polystyrene containing 0.1% Formulation 339. Weigh 10 g of the sample, crush it with a freeze pulverizer, dissolve the sample in 200 mL of DMSO, keep the reaction temperature at 20 °C, add 50 mL of DMSO solution containing 1 mL of chlorosulfonic acid, and react for 50 min. After the reaction was completed, 250 mL of distilled water was added to the solution, shaken vigorously in a separatory funnel for 10 min, and the aqueous phase was separated. The aqueous phase solution was poured into a supercritical extraction kettle, and the supercritical CO with a temperature of 110 °C and a pressure of 16 MPa was introduced. 2 , extracted for 20 min, filtered to remove the solid, and the filtrate was the sulfonated preparation 339. Using LC-MS detection, the detection conditions were the same as in Example 1, the retention time of the sulfonated preparation 339 was 7.6 min, and the M-1 peak was 213. Using dibutyl phthalate as an internal standard, the c...
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