High-Performance Liquid Chromatography-Tandem Mass Spectrometry For Determination Of Poracin Residues In Rice And Millet
Advanced analytical method for detecting patulin in rice and millet, optimizing extraction, purification, and ensuring food safety with high accuracy.
By optimizing the extraction solvent and its volume, ultrasonic time and adsorbent, a fast, simple and accurate analytical method for the determination of patulin in rice and millet was established. Acetonitrile was used as the extraction solvent, and the ethylenediamine-N-propylsilane (PSA) adsorbent was used for purification. The supernatant was analyzed after passing through the membrane, and the multiple reaction monitoring (MRM) mode was used in the electrospray ionization (ESI) mode. Determination. The results showed that patulin showed good linearity in the range of 0.1~100.0 ¦Ìg/L, and the correlation coefficient was not less than 0.999 0. The detection limit of patulin in rice is 0.03 ¦Ìg/kg, the lower limit of quantitation is 0.1 ¦Ìg/kg, the recovery rate is 88.3%~91.5%, and the relative standard deviation (RSD) is 2.3%~6.0%; The detection limit of mycin is 0.1 ¦Ìg/kg, the lower limit of quantification is 0.3 ¦Ìg/kg, the recovery rate is 92.7%~103.8%, and the RSD is 2.2%~6.9%, which meets the requirements of trace analysis. The collected rice and millet samples were analyzed using this method, and no patulin was detected.
Introduction to Patulin Detection in Food Products
The detection and quantification of patulin, a mycotoxin found in various food products, pose significant challenges due to its potential health risks. Recent advancements in analytical methodologies have led to the development of a rapid, straightforward, and precise approach for determining the presence of patulin in rice and millet. This paper outlines the optimization of various parameters, including the extraction solvent and volume, ultrasonic time, and adsorbent, culminating in an efficient method leveraging acetonitrile for extraction and ethylenediamine-N-propylsilane (PSA) for purification.
Optimization of Extraction and Purification Methods
The method’s efficiency hinges on the meticulous selection of acetonitrile as the extraction solvent, renowned for its efficacy in isolating patulin from complex matrices such as rice and millet. Following extraction, the purification process employs PSA, an adsorbent that significantly enhances the purity of the sample by removing interfering substances, thus ensuring the accuracy of subsequent analyses.
Analytical Procedure and Method Validation
Post-purification, the sample undergoes analysis through a membrane, with the supernatant being subjected to scrutiny under multiple reaction monitoring (MRM) mode within the electrospray ionization (ESI) spectrum. This sophisticated approach allows for the precise identification and quantification of patulin, boasting an impressive linear range of 0.1 to 100.0 μg/L and a correlation coefficient exceeding 0.999, indicative of the method’s reliability and reproducibility.
Sensitivity and Accuracy in Patulin Detection
The method demonstrates exceptional sensitivity and accuracy, with a detection limit for patulin in rice at 0.03 μg/kg and a quantification lower limit of 0.1 μg/kg. The recovery rates ranged from 88.3% to 91.5%, with a relative standard deviation (RSD) between 2.3% and 6.0%. Similarly, for millet, the detection limit was identified at 0.1 μg/kg, with a quantification lower limit of 0.3 μg/kg. The recovery rates in millet were slightly higher, ranging from 92.7% to 103.8%, and the RSD spanned from 2.2% to 6.9%, underscoring the method’s efficacy and robustness for trace analysis in both matrices.
Application and Efficacy of the Developed Method
The developed method was applied to analyze collected samples of rice and millet, yielding no detectable levels of patulin, thereby confirming the method’s capability in screening for this mycotoxin. This not only attests to the potential safety of the analyzed samples but also highlights the method’s practical applicability in ensuring food safety.
Conclusion and Implications for Food Safety
In conclusion, the establishment of this analytical method marks a significant stride towards enhancing food safety protocols. By optimizing critical parameters such as the extraction solvent, ultrasonic time, and adsorbent, this method offers a rapid, simple, and accurate solution for the determination of patulin in rice and millet. Its high sensitivity, precision, and recovery rates meet the stringent requirements of trace analysis, making it an invaluable tool in the ongoing efforts to safeguard public health against the risks posed by mycotoxins in food products.
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Original research was done by Wang Fuhua, Shi Jieping, Zhao Yarong, Huang Jianxiang
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