Li An-Ping, Shi Yan-Ping
CAS Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences (CAS), 18 Tianshui Middle Road, Lanzhou 730000, PR China.
Gansu Institute for Drug Control, Key Laboratory for Quality Control of Chinese Medicinal Materials and Decoction Pieces, National Medical Products Administration (NMPA), Lanzhou 730000, PR China.
J AOAC Int. 2022 Dec 22;106(1):192-204. doi: 10.1093/jaoacint/qsac088.
Farfarae Flos (FF) is a frequently used traditional herbal medicine with outstanding antitussive actions. The adulteration of FF decoction pieces is common.
This study aimed to study the effect of adulteration on the safety and quality of FF decoction pieces.
The proportion of impurities was conducted by cone quartering method. A simple and accurate ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was established to simultaneous determinate three pyrrolizidine alkaloids (PAs) as endogenous toxic compounds in FF. The traditional medicinal parts (flower bud), impurities (pedicel and rhizome) and unselected samples were determined respectively. The values of estimated daily intake (EDI) and margin of exposure (MOE) were used for risk assessment.
Twenty batches of samples were collected from different habitats, and the proportion of impurities ranged from 17.51% to 41.27%. Pedicel and rhizome were the main impurities, accounting for more than 87.40% of the total impurities. The content of PAs in impurities was significantly higher. The EDI value range was 5.34 to 16.59 μg/kg bw/day, which was much higher than the standard safety value of 7.00 × 10-3 μg/kg bw/day. The MOE values ranges for life long time and shorter exposure were 14.29 to 44.37 and 371.53 to 1153.63, respectively, indicating that at least 80% of the samples had safety risks. Correlation analysis showed that the proportion of adulterated impurities had significant correlation with the values of EDI and MOE.
Adulteration of non medicinal parts may significantly increase the risk of medications of FF decoction pieces.
This study provides an efficient methodology reference for the control of PAs and a basis for adulteration to affect the safety and quality of FF decoction pieces.
款冬花是一种常用的传统草药，具有出色的止咳作用。款冬花饮片掺假现象普遍。
本研究旨在探讨掺假对款冬花饮片安全性和质量的影响。
采用四分法测定杂质比例。建立了一种简单准确的超高效液相色谱串联质谱法（UHPLC-MS/MS），同时测定款冬花中三种吡咯里西啶生物碱（PAs）作为内源性有毒化合物。分别测定传统药用部位（花蕾）、杂质（花梗和根茎）和未筛选样品。采用估计每日摄入量（EDI）和暴露边际（MOE）值进行风险评估。
从不同产地收集了20批样品，杂质比例在17.51%至41.27%之间。花梗和根茎是主要杂质，占总杂质的87.40%以上。杂质中PAs的含量显著更高。EDI值范围为5.34至16.59μg/kg体重/天，远高于标准安全值7.00×10-3μg/kg体重/天。终身暴露和短期暴露的MOE值范围分别为14.29至44.37和371.53至1153.63，表明至少80%的样品存在安全风险。相关性分析表明，掺假杂质比例与EDI和MOE值具有显著相关性。
非药用部位掺假可能显著增加款冬花饮片用药风险。
本研究为PAs的控制提供了一种有效的方法学参考，也为掺假影响款冬花饮片安全性和质量提供了依据。
