Method for determining nitrite in food by employing headspace-gas chromatography/mass spectrography
A gas chromatography and nitrite technology, applied in the field of food safety detection, can solve the problems of strong interference in absorption measurement, high detection limit, complicated operation, etc., and achieve high sensitivity and accuracy, improved detection efficiency, and repeatability. Good results
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Embodiment 1
[0060] Example 1: Establishment of a method for determining nitrite in food using headspace-gas chromatography / mass spectrometry of the present invention 1. Extraction step
[0061] Weigh 1g of food sample and put it into a centrifuge tube, add 2.5ml of zinc acetate solution (concentration of 219g / L), 2.5ml of potassium ferrocyanide solution (concentration of 109g / L), add 15ml of pure water, shake and mix thoroughly. After mixing, ultrasonic extraction was performed for 20 min, filtered with filter paper, and the filtrate was collected for use.
[0062] Take 5ml of the deproteinized filtrate, 5ml of 1% sulfuric acid solution and 0.1% sodium cyclamate solution in the headspace bottle, and quickly cover the bottle for headspace-gas chromatography / mass spectrometry (HS-GC / MS) analysis; The response peak area of cyclohexene corresponds to the nitrite content as a calibration curve for quantitative analysis.
[0063] 2. Instrument parameters and measurement conditions
[0064] ...
Embodiment 2
[0115] Example 2: Determination experiment of detection limit, linear range and recovery range of the method of the present invention
[0116] According to the method in Example 1, the detection limit, precision and recovery rate of this method were determined. Table 2 is the regression equation and correlation coefficient of sodium nitrite standard.
[0117] Table 2
[0118] name
standard curve line
Sodium nitrite
Y=178314X-6528.8
0.9987
[0119] Image 6 is the correlation coefficient plot of nitrite concentration and response value. At the concentration of 0.1mg / L-5mg / L, the response value of sodium nitrite standard has a good linear relationship with the mass concentration. The correlation coefficient is greater than 0.998. The lower limit of detection (LOD) of the compounds was determined based on a 3-fold signal-to-noise ratio (S / N), and the limit of quantitative detection for nitrite in food was 100 ...
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