A liquid chromatography detection method for chlorphenesin in toy materials, comprising the following steps:
(1) Prepare standard solution and fit standard curve equation
Weigh 0.05g (accurate to 0.0001g) of chlorphenesin, add methanol-water (50:50, v/v), ultrasonically dissolve and transfer to a 50mL volumetric flask, dilute to the mark with methanol-water solution, shake Evenly, it was made into a standard stock solution with a mass concentration of 1000mg/L;
Pipette 5.0mL of 1000mg/L standard stock solution into a 100mL volumetric flask, dilute to the mark with methanol-water (50:50, v/v) solution, shake well, and make an intermediate working solution with a mass concentration of 50mg/L standard solution;
Pipette 0.20, 1.00, 2.00, 10.0mL of chlorphenesin intermediate working standard solution and 1.00, 2.50, 5.00mL of standard stock solution into 10mL volumetric flask, dilute with methanol-water (50:50, v/v) To the scale, shake well to obtain a series of concentration standard solutions with mass concentrations of 1.00, 5.00, 10.0, 50.0, 100, 250 and 500;
Take the peak area as the ordinate (Y), and the mass concentration in the standard solution as the abscissa (X) to carry out linear regression, and obtain the regression equation of chlorphenesin as Y=4.11(e+003)X-1.46(e+004) .
(2) Sample processing
Weigh 1.0g of the sample (accurate to 0.0001g) into a 10mL stoppered colorimetric tube, add the extraction solution (methanol-water (50:50, v/v)) to the mark and seal it with a parafilm, vortex shake for 1.0min , ultrasonically extracted for 20-35min, then filtered through a 0.22μm filter membrane, and the filtrate was used as the sample solution to be tested;
(3) Chromatographic detection
Carry out gradient elution with methanol-water as mobile phase according to Table 1, adopt C-18 column as chromatographic column (100mm * 2.1mm, 1.7 μ m), with photodiode array (PDA) detector, detection wavelength 280nm (chlorophenglycine Ether detection wavelength), flow rate 0.2mL/min, column temperature 30°C, injection volume 1 μL, and substitute the measured peak area into the regression equation of step (1) to obtain the mass concentration of chlorphenesin in the sample.
