A method for detecting mineral oil in chili oil by gas chromatography
A gas chromatography and mineral oil technology, applied in separation methods, chemical instruments and methods, measuring devices, etc., can solve the problems of complex operation, cumbersome steps, poor accuracy, etc., achieve high resolution, avoid baseline drift, and complete peak output Effect
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Embodiment 1
[0031] Preparation of SPE column:
[0032] (1) Weigh 49.5g of silica gel into a 250mL round-bottomed flask with an outer wall wrapped in aluminum foil, and add 50mL of 1% silver nitrate solution dropwise to the flask, mix it with a rotary evaporator for 3h, let it stand for 12h, and put it in 125 Dry in an oven at ℃ for 12 hours to obtain silver nitrate-impregnated silica gel. Mix 32 g of silver nitrate-impregnated silica gel with 68 g of activated silica gel to obtain 0.3% silver nitrate silica gel. Store in a desiccator away from light and use within 2 weeks;
[0033] (2) Take a 5mL glass syringe tube (8cm×13mm) whose outer layer is wrapped with aluminum foil, put a round glass fiber filter paper in the bottom, and fill the lumen with 3g of 0.3% silver nitrate silica gel, tap and compact , and then lay a layer of glass fiber filter paper to obtain the SPE column.
Embodiment 2
[0035]The method that gas chromatography detects mineral oil in capsicum oil, comprises the following steps:
[0036] (1) Prepare gas chromatography working conditions, chromatographic column: Agilent DB-5HT, 15m×0.25mm×0.1μm; GC analysis conditions: initial temperature 40°C, keep for 5min, raise temperature to 80°C at 8°C / min, keep for 2min , then raise the temperature to 290°C at 5°C / min, keep for 2min, and finally raise the temperature to 330°C at 10°C / min, keep for 2min; the temperature of the injection port is 300°C; the injection volume is 1μL; splitless injection; the FID temperature is 280°C , the hydrogen flow rate is 30mL / min, the air flow rate is 400mL / min, the compensation gas is nitrogen, and the flow rate is 25mL / min;
[0037] (2) Use a 100 μL pipette to accurately measure C 7 ~C 40 Put the n-paraffin mixed standard solution in a 5mL volumetric flask, dilute it to volume with n-hexane and carry out isocratic dilution to obtain a series of concentrations of 0.32...
Embodiment 3
[0054] Spike recovery experiment
[0055] (1) On the basis of Example 2, take chili oil as the sample matrix, add C 7 ~C 40 Normal paraffin mixed standard solution carries out standard addition recovery experiment, and addition level is respectively 120, 160 and 200mg / kg, carries out chromatographic detection, obtains chromatogram data (such as image 3 As shown, wherein, a is the addition amount of 120mg / kg; b is the addition amount of 160mg / kg; c is the addition amount of 200mg / kg), calculate the standard addition recovery (as shown in Table 3). The results showed that the recovery rate of standard addition was between 90.2% and 118.4%, which could meet the requirements of analysis and detection.
[0056] table 3
[0057]
[0058] The method for gas chromatography detection of mineral oil in capsicum oil provided by the invention can make the peak separation of each component more complete and clear through the purification of mineral oil extract in capsicum oil and th...
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