Method for determining residues of seven sulfonamide antibiotics in sediment sample
A sediment and sulfonamide technology is applied in the field of determination of 7 kinds of sulfonamide antibiotic residues in sediment samples, which can solve the problems of poor anti-interference ability and insufficient sensitivity, and achieve the improvement of accuracy, high detection sensitivity and grinding precision. Effect
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Embodiment 1
[0041] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:
[0042] S1: Sample Collection:
[0043] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;
[0044] S2: Sample pretreatment:
[0045] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1400psi , temperature 70°C, keep 10min, 60% flushing volume, flush 50s, use methanol / acetone (50 / 50, V / V) to ob...
Embodiment 2
[0059] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:
[0060] S1: Sample Collection:
[0061] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;
[0062] S2: Sample pretreatment:
[0063] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1500psi , the temperature is 80°C, keep 10min, 60% of the washing volume, wash for 60s, use methanol / acetone (5...
Embodiment 3
[0077] A method for determining residues of 7 kinds of sulfa antibiotics in sediment samples, 7 kinds of sulfa antibiotics include sulfadiazine, sulfamethoxazole, sulfamethizole, sulfathiazole, sulfamethazine, sulfabenzopyrazole, sulfamethazine pyrimidine, comprising the steps of:
[0078] S1: Sample collection:
[0079] Collect sediment samples at the sampling point, remove impurities, freeze-dry, put them in a grinding storage device for grinding and store them for testing. The grinding conditions are 60-mesh sieve, and the storage temperature is -20°C;
[0080] S2: Sample pretreatment:
[0081] Accurately weigh 5±0.01g of the above-mentioned ground sediment sample, mix it with 2g±0.05g of diatomaceous earth, put it into a 33ml extraction pool, and use Dionne 300 Accelerated Solvent Extraction (ASE) system for extraction, the extraction condition is a pressure of 1600psi , the temperature is 90°C, keep 10min, 60% of the washing volume, wash for 70s, use methanol / acetone (5...
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