High-performance-liquid-chromatography detection method for methylene blue in aquaculture water

Abstract

The invention discloses a high-performance-liquid-chromatography detection method for methylene blue in aquaculture water. The method comprises: pre-processing the aquaculture water, performing extraction by employing dichloromethane, performing vacuum-pumping condensation purification by employing a rotary evaporator, detecting by employing a liquid chromatogram-ultraviolet detector, and employing an external standard method to perform quantitative analysis. The method is convenient to operate, relatively good in repeatability, accurate in qualification and relatively high in recovery rate, and is capable of rapidly analyzing the methylene blue content in aquaculture water.

Description

technical field

[0001] The invention relates to the technical field of environmental quality and safety detection, in particular to a high performance liquid chromatography detection method for methylene blue in aquaculture water. Background technique

[0002] Methylene blue belongs to a chemical indicator, industrial dye, biological dye and drug, and its toxicity is lower than that of malachite green. In recent years, it has been widely used in aquatic product cultivation as a substitute for banned drugs such as malachite green and nitrofuran It can prevent streptochytridosis, saprolegniasis and parasitic diseases caused by fungi. It is often used in aquaculture to treat saprolegniasis and to disinfect the environment of aquaculture water. Extensive use or abuse of methylene blue will have certain toxic and side effects on aquaculture aquatic organisms, and it is difficult to control the concentration of the drug in actual production, resulting in the accumulation of a cert...

Examples

Embodiment 1

[0026] (1) Water sample pretreatment: After collecting 500 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0027] (2) Extraction and purification: Select a 250 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 100 mL of the filtrate and transfer it to a 250 mL separatory funnel, add 40 mL of chromatographically pure dichloromethane for extraction, shake for 1 min and then statically After standing for 20 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 40 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-tip...

Embodiment 2

[0035] (1) Water sample pretreatment: After collecting 1000 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0036] (2) Extraction and purification: Select a 500 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 250 mL of the filtrate and transfer it to a 500 mL separatory funnel, add 50 mL of chromatographically pure dichloromethane for extraction, shake for 2 minutes and then let it stand After 30 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 45 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-tipped st...

Embodiment 3

[0044] (1) Water sample pretreatment: After collecting 1000 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0045] (2) Extraction and purification: Select a 500 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 250 mL of the filtrate and transfer it to a 500 mL separatory funnel, add 60 mL of chromatographically pure dichloromethane for extraction, shake for 1 min and then statically After standing for 20 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 40 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-ti...

technical field

[0001] The invention relates to the technical field of environmental quality and safety detection, in particular to a high performance liquid chromatography detection method for methylene blue in aquaculture water. Background technique

[0002] Methylene blue belongs to a chemical indicator, industrial dye, biological dye and drug, and its toxicity is lower than that of malachite green. In recent years, it has been widely used in aquatic product cultivation as a substitute for banned drugs such as malachite green and nitrofuran It can prevent streptochytridosis, saprolegniasis and parasitic diseases caused by fungi. It is often used in aquaculture to treat saprolegniasis and to disinfect the environment of aquaculture water. Extensive use or abuse of methylene blue will have certain toxic and side effects on aquaculture aquatic organisms, and it is difficult to control the concentration of the drug in actual production, resulting in the accumulation of a cert...

Examples

Embodiment 1

[0026] (1) Water sample pretreatment: After collecting 500 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0027] (2) Extraction and purification: Select a 250 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 100 mL of the filtrate and transfer it to a 250 mL separatory funnel, add 40 mL of chromatographically pure dichloromethane for extraction, shake for 1 min and then statically After standing for 20 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 40 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-tip...

Embodiment 2

[0035] (1) Water sample pretreatment: After collecting 1000 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0036] (2) Extraction and purification: Select a 500 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 250 mL of the filtrate and transfer it to a 500 mL separatory funnel, add 50 mL of chromatographically pure dichloromethane for extraction, shake for 2 minutes and then let it stand After 30 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 45 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-tipped st...

Embodiment 3

[0044] (1) Water sample pretreatment: After collecting 1000 mL of water sample to the laboratory, immediately use a 0.45 μm filter membrane for suction filtration treatment, and transfer the filtrate obtained by suction filtration to a sample bottle.

[0045] (2) Extraction and purification: Select a 500 mL separatory funnel for leak detection and place it on the funnel stand, accurately measure 250 mL of the filtrate and transfer it to a 500 mL separatory funnel, add 60 mL of chromatographically pure dichloromethane for extraction, shake for 1 min and then statically After standing for 20 min, when the liquid in the separatory funnel was stable and obvious stratification appeared, the dichloromethane in the lower layer was transferred to a 100 mL rotary evaporator, and concentrated to dryness in a rotary evaporator at 40 °C under vacuum. After removing the rotary evaporator, accurately add 1.0 mL of methanol to the rotary evaporator to dissolve the residue, and use a rubber-ti...

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