Zhang Rong, Yang Ya-Ling, Deng Ai-Ping, Kang Li-Ping, Cheng Ming-En, Kang Chuan-Zhi, Guo Lan-Ping
School of Pharmacy, Anhui University of Chinese Medicine Hefei 230012, China State Key Laboratory Base of Daodi Herbs, National Resource Center for Chinese Materia Medica, China Academy of Chinese Medical Sciences Beijing 100700, China.
State Key Laboratory Base of Daodi Herbs, National Resource Center for Chinese Materia Medica, China Academy of Chinese Medical Sciences Beijing 100700, China.
Zhongguo Zhong Yao Za Zhi. 2023 Feb;48(3):660-671. doi: 10.19540/j.cnki.cjcmm.20221031.301.
Lilii Bulbus is a commonly used Chinese herbal medicine with both medicinal and edible values, while the market products usually has the problem of sulfur fumigation. Therefore, the quality and safety of Lilii Bulbus products deserve attention. In this study, ultra-high performance liquid chromatography-time of flight-tandem mass spectrometry(UPLC-Q-TOF-MS/MS) was combined with principal component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) to analyze the differential components of Lilii Bulbus before and after sulfur fumigation. We identified ten markers generated after sulfur fumigation, summarized their mass fragmentation and transformation patterns, and verified the structures of phenylacrylic acid markers of sulfur fumigation. At the same time, the cytotoxicity of the aqueous extracts of Lilii Bulbus before and after sulfur fumigation was evaluated. The results showed that in the concentration range of 0-800 mg·L~(-1), the aqueous extract of Lilii Bulbus after sulfur fumigation had no significant effect on the viability of human liver LO2 cells, human renal proximal tubular HK-2 cells, and rat adrenal pheochromocytoma PC-12 cells. Moreover, the viability of the cells exposed to the aqueous extract of Lilii Bulbus before and after sulfur fumigation showed no significant difference. This study identified phenylacrylic acid and furostanol saponins as markers of sulfur-fumigated Lilii Bulbus for the first time, and made clear that proper sulfur fumigation of Lilii Bulbus would not produce cytotoxicity, providing a theoretical basis for the rapid identification and quality and safety control of sulfur-fumigated Lilii Bulbus.
百合是一种常用的具有药用和食用价值的中药材,而市场上的产品通常存在硫熏问题。因此,百合产品的质量和安全性值得关注。本研究采用超高效液相色谱-飞行时间串联质谱(UPLC-Q-TOF-MS/MS)结合主成分分析(PCA)和正交偏最小二乘法判别分析(OPLS-DA),分析硫熏前后百合的差异成分。我们鉴定了硫熏后产生的10个标志物,总结了它们的质谱裂解和转化模式,并对硫熏苯丙烯酸类标志物的结构进行了确证。同时,评价了硫熏前后百合水提取物的细胞毒性。结果表明,在0800 mg·L(-1)浓度范围内,硫熏后百合水提取物对人肝LO2细胞、人肾近端小管HK-2细胞和大鼠肾上腺嗜铬细胞瘤PC-12细胞的活力无显著影响。此外,硫熏前后百合水提取物作用的细胞活力无显著差异。本研究首次鉴定出苯丙烯酸类和呋甾烷醇皂苷类为硫熏百合的标志物,并明确了百合适度硫熏不会产生细胞毒性,为硫熏百合的快速鉴别及质量与安全性控制提供了理论依据。