Shipin yu jixie (Jan 2024)
Determination of cholic acid and derivative residues in eggs by UPLC-MS/MS
Abstract
Objective: The pretreatment method of through-type solid-phase extraction was improved to be coupled with ultra performance liquid chromatography tandem mass spectrometry for detection of cholic acid,deoxycholic acid and dehydrochloric in eggs. Methods: The samples were extracted by methanol and purified by PRiME HLB,then separated on C18(100 mm×2.1 mm,3.0 μm) column with methanol-0.1% ammonia as the mobile phase for gradient elution. Meanwhile,the samples were quantified by external standard with negative ion select reaction monitoring (SRM) mode. Results: The results showed that the linear relationships of cholic acid (CA),deoxycholic acid (DCA) and dehydrochloric acid(DHCA) were good in the range from 0.5 ng/mL to 500 ng/mL(R2>0.999). The detection limits and quantitative limits of CA,DCA and DHCA were 1.0 μg/kg and 3.3 μg/kg. The average recovery of CA,DCA and DHCA from 1.0~10 μg/kg were 93.7%~102.5%,with the RSD of 1.8%~9.2%. 30 batches of randomly selected eggs were tested, and cholic acid was detected in all 28 batches of samples. Conclusion: This method is rapid with high sensitivity,accuracy,and it can be used as a method for the determination of cholic acid and derivative residues in eggs.
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