Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization
Puberulic acid (PA) is a mycotoxin produced by a species of <i>Penicillium</i>. It has received widespread attention as a significant contributor to the reported fatalities associated with red yeast rice dietary supplements. However, the detection of PA, especially at low concentration l...
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MDPI AG
2024-12-01
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| author | Hui-Qin Pan Rui Feng Yan-Nan Tan Xiao-Ya Qin Yi-Min Cao Xiu-Hong Mao Qing Hu Heng Zhou |
| author_facet | Hui-Qin Pan Rui Feng Yan-Nan Tan Xiao-Ya Qin Yi-Min Cao Xiu-Hong Mao Qing Hu Heng Zhou |
| author_sort | Hui-Qin Pan |
| collection | DOAJ |
| description | Puberulic acid (PA) is a mycotoxin produced by a species of <i>Penicillium</i>. It has received widespread attention as a significant contributor to the reported fatalities associated with red yeast rice dietary supplements. However, the detection of PA, especially at low concentration levels, poses a considerable challenge, with no detection methods reported thus far. Here, we present a simple and sensitive derivatization-based LC-MS/MS method, requiring no purification processes, for determination of PA in the red yeast rice. The methylating derivatization with trimethylsilyldiazomethane (TMSCHN<sub>2</sub>) was performed to enhance its analytical performance. To achieve optimal detection sensitivity, the amount of solvent and TMSCHN<sub>2</sub> for the derivatization reaction, along with the reaction time, were individually optimized. Moreover, sample extraction solvent was carefully chosen to improve recoveries in real sample analyses. Comparatively, the proposed LC-MS/MS method achieved a superior detection sensitivity, over 100-fold higher than that of the liquid chromatography method. A good linear relationship within the concentration range of 5 ng/mL to 200 ng/mL (with a linear correlation coefficient of 0.99952) was demonstrated by the method validation. The average recovery rate was between 82.2% and 84.2%, and the repeatability (RSD of 2.1% to 10.4%, n = 6) was satisfactory. The derivatized PA remained stable within 48 h. The limit of detection and the limit of quantification could reach 2 μg/kg and 50 μg/kg, respectively. As a result, the method was successfully applied to detect PA in over 42 batches of the red yeast rice samples. It indicated a low risk of PA contaminations in the red yeast rice products made in China. Furthermore, its application to the other health food products containing red yeast rice demonstrated the applicability of the established method. |
| format | Article |
| id | doaj-art-7c4f9fc91dcb47d8803be612d7c5f862 |
| institution | Kabale University |
| issn | 2072-6651 |
| language | English |
| publishDate | 2024-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Toxins |
| spelling | doaj-art-7c4f9fc91dcb47d8803be612d7c5f8622025-01-24T13:51:10ZengMDPI AGToxins2072-66512024-12-011711110.3390/toxins17010011Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn DerivatizationHui-Qin Pan0Rui Feng1Yan-Nan Tan2Xiao-Ya Qin3Yi-Min Cao4Xiu-Hong Mao5Qing Hu6Heng Zhou7NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaNMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, 1500 Zhangheng Road, Shanghai 201203, ChinaPuberulic acid (PA) is a mycotoxin produced by a species of <i>Penicillium</i>. It has received widespread attention as a significant contributor to the reported fatalities associated with red yeast rice dietary supplements. However, the detection of PA, especially at low concentration levels, poses a considerable challenge, with no detection methods reported thus far. Here, we present a simple and sensitive derivatization-based LC-MS/MS method, requiring no purification processes, for determination of PA in the red yeast rice. The methylating derivatization with trimethylsilyldiazomethane (TMSCHN<sub>2</sub>) was performed to enhance its analytical performance. To achieve optimal detection sensitivity, the amount of solvent and TMSCHN<sub>2</sub> for the derivatization reaction, along with the reaction time, were individually optimized. Moreover, sample extraction solvent was carefully chosen to improve recoveries in real sample analyses. Comparatively, the proposed LC-MS/MS method achieved a superior detection sensitivity, over 100-fold higher than that of the liquid chromatography method. A good linear relationship within the concentration range of 5 ng/mL to 200 ng/mL (with a linear correlation coefficient of 0.99952) was demonstrated by the method validation. The average recovery rate was between 82.2% and 84.2%, and the repeatability (RSD of 2.1% to 10.4%, n = 6) was satisfactory. The derivatized PA remained stable within 48 h. The limit of detection and the limit of quantification could reach 2 μg/kg and 50 μg/kg, respectively. As a result, the method was successfully applied to detect PA in over 42 batches of the red yeast rice samples. It indicated a low risk of PA contaminations in the red yeast rice products made in China. Furthermore, its application to the other health food products containing red yeast rice demonstrated the applicability of the established method.https://www.mdpi.com/2072-6651/17/1/11red yeast ricepuberulic acidLC-MS/MSprecolumn derivatizationmethylation |
| spellingShingle | Hui-Qin Pan Rui Feng Yan-Nan Tan Xiao-Ya Qin Yi-Min Cao Xiu-Hong Mao Qing Hu Heng Zhou Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization Toxins red yeast rice puberulic acid LC-MS/MS precolumn derivatization methylation |
| title | Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization |
| title_full | Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization |
| title_fullStr | Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization |
| title_full_unstemmed | Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization |
| title_short | Determination of Puberulic Acid in Monascus-Fermented Red Yeast Rice by LC-MS/MS Combined with Precolumn Derivatization |
| title_sort | determination of puberulic acid in monascus fermented red yeast rice by lc ms ms combined with precolumn derivatization |
| topic | red yeast rice puberulic acid LC-MS/MS precolumn derivatization methylation |
| url | https://www.mdpi.com/2072-6651/17/1/11 |
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