OBJECTIVE

2

To establish a method for the content determination of patulin in Citri Grandis Exocarpium.

METHODS

2

High-performance liquid chromatography-triple quadrupole mass spectrometer（HPLC-MS/MS）was used for the analysis. After water-soluble dispersion and pectinase enzymolysis， the Citri Grandis Exocarpium sample was extracted by acetonitrile with high-speed homogenated. The extracted solution was conducted dispersive solid phase extraction by mixing powder of MgSO

4

and NaAC （4∶1，

m

/

m

），then purified on SHIMSEN 228 solid phase purification column. Water acetonitrile was used as mobile phase， and the Shim-pack XR-ODS column was used to separate the target compound. And it was detected by electrospray ionization in the negative mode under multiple reaction monitoring， and quantified by the external standard method with matrix-matched standard correction curves.

RESULTS

2

Patulin showed good linear correlation in the concentration from 5 to 200 ng/mL （

r

＝0.999 6）. RSDs of precision， reproducibility and stability tests （12 h） were all lower than 6％. The average recoveries at low， medium， high concentrations were 83.9%， 92.08%， 92.21%， respectively （RSDs were 11.09%， 5.53%， 1.75%， respectively）. The limit of quantitation was 6 μg/kg and limit of detection was 3 μg/kg. Patulin was not detected in 20 batches of samples.

CONCLUSIONS

2

Established method can be used for the rapid detection and accurate quantification of patulin in Citri Grandis Exocarpium， which can provide experimental basis and method for safety study and quality control of Citri Grandis Exocarpium.