Method for detecting clenbuterol in pig hair
A detection method, the technology of clenbuterol, applied in the detection field, can solve the problems of short drug residue cycle, real-time tracking and monitoring of difficult drug residues, false positives, etc., and achieve good detection effect, good impurity removal effect, and easy operation Effect
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Embodiment 1
[0025] The preparation of embodiment 1CLE standard substance
[0026] Using water as a solution, prepare CLE standards with a content of 0.25ppm, 0.5ppm1ppm2ppm4ppm8ppm and 16ppm respectively, using a B&W TEK iRaman spectrometer, 780nm excitation light, and using instrument quantitative analysis software to make a standard curve for the concentration, such as figure 1 shown. It has a good linear relationship in the range of 0-16ppm.
Embodiment 2
[0027] Example 2 pig hair to be tested
[0028] 1. Hair digestion: Weigh 0.200g hair and add 4ml 1 molar NaOH, digest at 80°C for 10 minutes, and centrifuge at 8000 rpm for 5 minutes. Pour off the supernatant, add 1 mL of 1M NaOH solution, centrifuge at 8000 rpm for 5 minutes, and combine the supernatant for use.
[0029] 2. Liquid-liquid extraction: Add 10ml of dichloromethane to the supernatant for liquid-liquid extraction. After static layering, take the lower layer of clear liquid, and then add 5ml of 0.1M HCl to the lower layer of liquid for extraction again. After static layering, take the upper layer The supernatant was subjected to SPE (solid phase extraction.
[0030] 3. Solid-phase extraction: Take a PCX solid-phase extraction column (Tianjin Bona Agel Technology Co., Ltd.), activate it with 5mL water and 5mL methanol, pass the sample extract through the column, and use 5mL water, 5mL methanol:water at a ratio of 1:1 Wash the column with the mixed solution of the m...
Embodiment 3
[0033] Example 3 Blank pig hair (determined as blank by other standard methods)
[0034] 1. Hair digestion: Weigh 0.200g hair and add 4ml 1 molar NaOH, digest at 80°C for 10 minutes, and centrifuge at 8000 rpm for 5 minutes. Pour off the supernatant, add 1 mL of 1M NaOH solution, centrifuge at 8000 rpm for 5 minutes, and combine the supernatant for use.
[0035] 2. Liquid-liquid extraction: Add 10ml of dichloromethane to the supernatant for liquid-liquid extraction. After static layering, take the lower layer of clear liquid, and then add 5ml of 0.1M HCl to the lower layer of liquid for extraction again. After static layering, take the upper layer The supernatant was subjected to SPE (solid phase extraction.
[0036] 3. Solid-phase extraction: take PCX solid-phase extraction column, activate it with 5mL water and 5mL methanol, pass the sample extract through the column, rinse the column with 5mL water, 5mL methanol:water mixed solution of 1:1, and drain the extraction column ...
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