Method for determining aflatoxin content in semen boitae
A kind of technology of aflatoxin and cypress kernel, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of beautiful peak shape, high response value and good reproducibility
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Embodiment 1
[0026] A method for measuring the content of aflatoxin in Baiziren, based on the IAC-HPLC-MS / MS method, the specific steps are:
[0027] (1) Sample extraction, take a cypress kernel sample, grind it with liquid nitrogen, extract, dilute, filter, and collect the supernatant;
[0028] (2) Purification and elution, take the sample solution and inject it into the immunoaffinity column; after the liquid is drained, wash with water, and discard all the eluent; after the liquid is drained, add methanol, collect the eluate and constant volume ; The eluent is transferred to the liquid phase vial after being filtered with a filter membrane as the sample to be tested for subsequent use;
[0029] (3) Establish a standard curve, dilute the aflatoxin mixed standard reference substance with methanol into different concentrations of aflatoxin mixed standard solutions, filter, and use the HPLC-MS / MS method to measure, take the peak area as the ordinate, and use four The mass concentration of ...
Embodiment 2
[0039] Embodiment 2 linear relationship investigation
[0040] Precisely draw the aflatoxin mixed standard solution, dilute it with methanol to a concentration of 1.0, 4.0, 8.0, 10.0, 30.0, 50.0, 80.0ug·kg -1 A series of standard solutions are filtered with a 0.22 μm organic filter membrane, and the sample injection is detected under the chromatographic conditions described in Example 1. With the aflatoxin concentration as the abscissa and the peak area as the ordinate, four kinds of aflatoxin standards are established respectively curve, to calculate the regression equation. The concentration with a signal-to-noise ratio of 3 was used as the detection limit, and the concentration with a signal-to-noise ratio of 10 was used as the limit of quantification. See Table 1 for the linear equations, linear ranges, correlation coefficients, detection limits, and quantitation limits of the four aflatoxins.
Embodiment 3
[0041] Embodiment 3 precision investigation
[0042] The prepared mass concentration is 15.0ug·kg -1 The aflatoxin mixed reference substance solution was continuously sampled 6 times according to the chromatographic conditions described in Example 1, and the RSD values of the peak areas of the four aflatoxins were measured, and the intraday precision was calculated; The RSD value of the aflatoxin peak area was used to calculate the day-to-day precision. The results showed that both the intra-day precision and the inter-day precision met the requirements, and the specific results are shown in Table 1.
[0043] Table 1 Relevant parameter list of four aflatoxin methodological investigations
[0044]
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