SPE-GC-MS测定生姜中黄樟素及其衍生物含量  

Determination of Safrole and Its Derivatives in Ginger by SPE-GC-MS

作　　者：张艳 陈子雷 郭长英 张文君 毛江胜 李慧冬 ZHANG Yan;CHEN Zilei;GUO Changying;ZHANG Wenjun;MAO Jiangsheng;LI Huidong(Institute of Agricultural Quality Standards and Testing Technology,Shandong Academy of Agricultural Sciences,Agricultural Quality and Safety Risk Assessment of Laboratory of the Ministry of Agriculture and Rural Areas(Jinan),Shandong Key Laboratory of Food Quality and Safety Testing Technology,Jinan 250100)

机构地区：[1]山东省农业科学院农业质量标准与检测技术研究所农业农村部产品质量安全风险评估实验室(济南)山东省食品质量与安全检测技术重点实验室,济南250100

出　　处：《食品工业》2022年第3期283-286,共4页The Food Industry

基　　金：国家农产品质量安全风险评估专项-生姜中生物毒素及典型农药残留风险评估(GJFP2019009);2019年度山东省农业农村厅地方标准计划项目-生姜中黄樟素类化合物的测定-气相色谱质谱法。

摘　　要：建立固相萃取-气相色谱-质谱(SPE-GC-MS)测定生姜中黄樟素及其衍生物的分析方法。样品经乙腈提取,氯化钠盐析后,采用PestiCarb/NH;柱净化,经DB-5MS毛细管色谱柱分离,选择离子监测模式(SIM)扫描测定,外标法定量。在0.01~1.0μg/mL的线性范围内,黄樟素及其衍生物均成良好线性关系,相关系数(R^(2))均大于0.995,检出限为3.2~8.5μg/kg;在50,100和500μg/kg 3个添加水平下,回收率为89.8%~107.8%,相对标准偏差(S_(RSD),n=6)为1.8%~6.9%。该方法准确度高,回收率好,可用于生姜样品中黄樟素及其衍生物的定性及定量分析,为市场监管和实验室检测提供技术支持。A solid phase extraction-gas chromatography-mass spectrometry(SPE-GC-MS)method for the determination of safrole and its derivatives in ginger was established.The sample was extracted with acetonitrile,salted out with sodium chloride,purified by a PestiCarb/NH;,and then separated by DB-5MS capillary column,selected ion scanning(SIM)mode,and external standard method was used for quantification.The linear relationship of safrole and its derivatives was good in the mass concentration range of 0.01-1.0μg/mL,and the correlation coefficient(R^(2))was greater than 0.995.The detection limit were 3.2-8.5μg/kg.At the spiked levels of 50,100 and 500μg/kg,the recoveries were 89.8%-107.8%,and the relative standard deviation(S_(RSD),n=6)were 1.8%-6.9%.This method had high accuracy and good recovery rate.It could be used for the qualitative and quantitative analysis of safrole and its derivatives in ginger samples,and providing new technical support for market supervision and laboratory testing.

关 键 词：固相萃取 气相色谱-质谱法 生姜 黄樟素及其衍生物 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]