A method for the determination of steroid hormones by ionic liquid homogeneous liquid-liquid extraction-high performance liquid chromatography

Abstract

The invention discloses an analysis method for determining six steroid hormones in milk and milk products by an ion liquid homogeneous-phase liquid-liquid extraction-high performance liquid chromatography. Conditions of ion liquid homogeneous-phase liquid-liquid extraction and a high performance liquid chromatograph are optimized through a standard addition recovery experiment with a certain concentration. Factors which influence extraction and sample preparation conditions are optimized, and optimum conditions for optimization are as follows: 70 micro-liters of ion liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate ion liquid is used as an extracting agent, 80 micro-liters of the ion liquid 1-hexyl-3-methyl imidazolium tetrafluoroborate ion liquid is used as an extracting agent, and 0.3593g / mL NH4PF6 is used as an ion pair reagent; the sample is extracted for 10s and centrifuged for 5min; the pH value of the sample solution is adjusted to be 3.0-5.0, and the concentration of NaCl is 7%; and the method is simple, convenient, rapid and environment-friendly, and is suitable for determining the six steroid hormones in the milk and the milk products.

Description

technical field [0001] The invention relates to an analysis method for determining steroid hormones in milk and dairy products by ionic liquid homogeneous liquid-liquid extraction-high performance liquid chromatography. Background technique [0002] Steroid hormones are a class of lipophilic, low molecular weight, and active compounds that have been widely used in animal husbandry to promote the growth of dairy animals and improve feed conversion efficiency, resulting in hormone residues in milk and dairy products. Hormone residues may endanger human health, such as causing endocrine-related tumors, birth and birth defects; inducing reproductive system cancer or leukemia; affecting the growth and development of infants and adolescents, causing precocious puberty, etc. Therefore, the EU and China ban the use of hormones in the production of animal food. As an important part of the daily diet of the general public, milk and dairy products have become a hot spot of concern for...

AI Technical Summary

Problems solved by technology

Colorimetry and thin-layer chromatography have relatively low sensitivity and are difficult to meet the requirements of the limit of quantification in modern analysis, and have been gradually eliminated; immunoassays are generally only aimed at the detection of a certain hormone component, which has its limitations; The process is complicated, and it is not conducive to a large number of popularization and application; gas chromatography can not be directly applied to the determination of hormones, because the boiling point of hormones is relatively high, it needs to be determined by gas chromatography after derivatization, and generally needs to be analyzed with mass spectrometry, The derivatization process increases the experimental steps, and the operation is more complicated; the high-performance liquid chromatography ultraviolet detection method is relatively easy to implement in the laboratory, and is suitable for the analysis of substances with high boiling points or poor thermal stability, so it is also suitable for the separation and determination of hormones, but the sensitivity and The selectivity is worse than that of HPLC-MS or HPLC-MS / MS, but HPLC-MS or HPLC-MS / MS also has its own disadvantages, such as relatively expensive instruments, high maintenance costs and the need for highly skilled operators , and there are also matrix effects in the experiment, etc.

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