| 基于QuEChERS-高效液相色谱－串联质谱法检测八角中莽草毒素的研究 |
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| 基金项目:国家自然科学基金（32061160473）；广东省食品质量安全重点实验室开放课题（2020KF006） |
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| 中文摘要:该文建立了八角中莽草毒素的高效液相色谱－串联质谱检测方法。样品在乙酸盐缓冲体系下经乙腈溶液提取，200 mg N-丙基乙二胺（PSA）和50 mg石墨化碳黑（GCB）净化后，使用Accucore aQ C18（2.1 mm × 150 mm，2.6 μm）柱分离，以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱，采用电喷雾离子源负离子模式（ESI－）及多反应监测模式（MRM）进行测定，外标法定量。结果显示，莽草毒素在1.0 ~ 100.0 ng/mL范围内线性关系良好，相关系数（r2）大于0.99。样品在0.02、0.20、0.40、1.00 mg/kg加标水平下的平均回收率为92.5% ~ 112%，相对标准偏差（RSD，n = 6）为1.1% ~ 6.0%，检出限和定量下限分别为0.006 mg/kg和0.02 mg/kg。用于市售八角中莽草毒素含量的测定，10份样品中有1份莽草毒素含量超过1.00 mg/kg。该方法简便、快速、灵敏、准确，可为八角的质量评价与真伪鉴别提供技术支撑。 |
| 中文关键词:八角 莽草毒素 QuEChERS 高效液相色谱-串联质谱 质量评价 |
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| Determination of Anisatin in Star Anise by High Performance Liquid Chromatography－Tandem Mass Spectrometry with QuEChERS Method |
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| Abstract:Chinese star anise（Illicium verum） is used as a spice in Asian while it is used as herbal remedy for infantile colic in America or Europe．Toxic Illicium species such as Japanese star anise （Illicium anisatum L.），resembling Chinese anise star，contain higher concentrations of sesquiterpene lactone neurotoxin named anisatin．Consumption of Chinese anise star contaminated or adulterated by such toxic Illicium species may cause fatal poisoning．However，it is difficult to distinguish between Chinese star anise and its adulterants just according to dried fruit appearance due to the morphological similarity．Therefore，it is of great significance to establish a method to identify Chinese star anise from its adulterants to ensure food safety．The aim of this work was to establish high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） with a quick，easy，cheap，effective，rugged and safe（QuEChERS） pretreatment for the determination of anisatin in star anise．The sample was extracted with acetonitrile in acetate buffer system．Then the extracted supernatant was purified with 200 mg of primary secondary amine （PSA） and 50 mg of graphitized carbon black（GCB）．The chromatographic separation was carried out on an Accucore aQ C18 column（2.1 mm × 150 mm，2.6 μm） by gradient elution，using methanol and 0.1% formic acid aqueous solution as the mobile phases．Anisatin was detected in negative electrospray ionization（ESI－） mode under multiple reaction monitoring（MRM） mode，then quantified by external standard method．The result showed that the calibration curve for anisatin had a good linear correlation in the range of 1.0－100.0 ng/mL，with a correlation coefficient（r2） higher than 0.99．At the four spiked levels of 0.02，0.20，0.40 and 1.00 mg/kg，the average recoveries ranged from 92.5% to 112%，with the relative standard deviations（RSDs） from 1.1% to 6.0%．The limit of detection（LOD） and the limit of quantification（LOQ） were 0.006 mg/kg and 0.02 mg/kg，respectively．The established method was applied to the determination of anisatin in 10 batches of Chinese star anise samples purchased from the local market，of which 1 batch was found containing anisatin exceeding 1.00 mg/kg．The result indicated that there was a potential adulteration risk of Chinese star anise in the market．This proposed method is simple，rapid，sensitive and accurate，and it could provide a technical support for the quality evaluation and authenticity discrimination on Chinese star anise. |
| Key Words:star anise anisatin QuEChERS high performance liquid chromatography-tandem mass spectrometry quality assessment |
| 引用本文：钟玉心，王宇，钱振杰，陈彦宏，张辉，王伟，何咏欣，杨嘉鑫威，龚海锟，徐振林.基于QuEChERS-高效液相色谱－串联质谱法检测八角中莽草毒素的研究[J].分析测试学报,2022,41(11):1690-1695. |
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