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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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| DOI： |
| KeyWord:star anise anisatin QuEChERS high performance liquid chromatography-tandem mass spectrometry quality assessment |
| Author | Institution |
| ZHONG Yu-xin，WANG Yu，QIAN Zhen-jie，CHEN Yan-hong，ZHANG Hui，WANG Wei，HE Yong-xin，YANG Jia-xin-wei，GONG Hai-kun，XU Zhen-lin |
1. Guangdong Provincial Key Laboratory of Food Quality and Safety，College of Food Science，South China Agricultural University，Guangzhou ，China;
2. Guangzhou Institute for Food Inspection， Guangzhou ，China;
3. Huangpu Customs Technical Center， Guangzhou ，China |
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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. |
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