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作 者:王立媛[1] 应英[1] 于村[1] 胡争艳[1] 王天娇[1] 吴平谷[1] WANG Li-yuan;YING Ying;YU Cun;HU Zheng-yan;WANG Tian-jiao;WU Ping-gu(Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 315001,China)
机构地区:[1]浙江省疾病预防控制中心,浙江杭州310051
出 处:《中国卫生检验杂志》2022年第24期2983-2985,2989,共4页Chinese Journal of Health Laboratory Technology
摘 要:目的 建立葱属植物中二烯丙基二硫醚(DATS)和二烯丙基三硫醚(DADS)的气相色谱分析方法。方法 样品经匀浆后,在60℃及pH值为7的条件下酶解,经90%乙醇溶液在60℃提取60 min,然后再用正己烷萃取。最后经DB-1毛细管色谱柱(30 m×0.25 mm, 0.25μm)分离,火焰光度检测器(FPD)检测,外标法定量。结果 本法在0.5μg/ml~10.0μg/ml,通过二次曲线拟合,DATS和DADS的相关系数均为0.999 7,方法的检出限分别为0.1 mg/kg和0.2 mg/kg,在0.5 mg/kg、2.5 mg/kg、7.5 mg/kg 3个加标水平,平均回收率为85.3%~92.4%,相对标准偏差(RSD)为3.97%~7.81%。采用此方法对20份新鲜葱属植物(包括大蒜、洋葱、韭菜、大葱、蒜苔)进行了测定,结果显示,大蒜中大蒜素含量(DATS和DADS之和)最高,其次是洋葱、韭黄,大葱和蒜苔中含量相对较低。结论 本法操作简单、快速、准确,灵敏度相对其他方法更高,适用于葱属类植物中大蒜素的定量测定。Objective This paper aims to establish a gas chromatographic method for the analysis of diallyl disulfide(DATS) and diallyl trisulfide(DADS) in allium plants. Methods The samples were homogenized and enzymatically digested under the conditions of 60℃and pH=7, and then the analytes were extracted with 90% ethanol solution at 60 ℃ for 60 min. After the extraction with n-hexane, the analytes were separated on a DB-1 capillary column(30 m×0.25 mm, 0.25 μm) and detected with a flame photometric detector(FPD). Quantification was based on external standard curves. Results The correlation coefficients(r) of DATS and DADS were both 0.999 7(quadratic curve fitting) within 0.5 μg/ml-10.0 μg/ml. The limits of detection of the method were 0.1 mg/kg and 0.2 mg/kg. The average recoveries at the three spiked levels of 0.5 mg/kg, 2.5 mg/kg and 7.5 mg/kg were within 85.3%-92.4% with the relative standard deviations(RSD) of 3.97%-7.81%. This method was applied to 20 fresh samples including garlic, onion, leek, shallot and garlic shoots and the results showed that the highest allicin content(sum of DATS and DADS) was found in garlic, followed by onion, leek and relatively lower in shallot and garlic shoots. Conclusion The method is simple, rapid, accurate and more sensitive than other methods, which is suitable for the quantitative determination of allicin in allium plants.
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