三氟化硼乙醚衍生-气相色谱-质谱联用法测定糕点中5种防腐剂  

Determination of 5 preservatives in pastry by boron trifluoride etheratederivation - gas chromatography mass spectrometry

作　　者：王立媛[1] 刘丛娟 胡争艳[1] 陈婧 吴平谷[1] 应英[1] WANG Li-yuan;LIU Cong-juan;HU Zheng-yan;CHEN Jing;WU Ping-gu;YING Ying(Zhejiang Provincial Center for Disease Control and Prevention,Zhejiang 310051,China;不详)

机构地区：[1]浙江省疾病预防控制中心,杭州310051 [2]温州医科大学生命科学院

出　　处：《中国卫生检验杂志》2023年第18期2206-2209,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立糕点中苯甲酸、山梨酸、富马酸、马来酸和己二酸的氟化硼乙醚衍生-气相色谱-质谱联用同时测定法。方法样品经V/V(1:1)盐酸酸化,乙腈涡旋萃取,正己烷除脂,弃去正己烷层,乙腈层氮吹至近干,甲醇溶解,用氟化硼乙醚衍生,正己烷提取,饱和氯化钠溶液洗涤,吸取正己烷层用气相色谱-质谱联用法(GC-MS)测定,水杨酸内标法定量。结果5种防腐剂在1.0μg/ml~50μg/ml内相关系数均>0.99,方法检出限为0.33 mg/kg~1.0 mg/kg,定量限为1.09 mg/kg~3.0 mg/kg,平均回收率为83.6%~109.19%,相对标准偏差为1.74%~8.77%(n=6)。结论该方法样品用量少,灵敏度高,操作简单快速,适用于糕点中多种防腐剂的同时测定。Objective This paper aims to establish a method for the simultaneous determination of benzoic acid,sorbic acid,fumaric acid,maleic acid,adipic acid in pastry by boron trifluoride etherate derivation-gas chromatography mass spectrometry.Methods The samples were acidified with hydrochloric acid V/V(1:1),and then the analytes were extracted with acetonitrile and defatted with n-hexane.The n-hexane layer was discarded,the acetonitrile layer was blown to nearly dry,dissolved in methanol,derived with boron fluoride ether,extracted with n-hexane,washed with saturated sodium chloride solution,the n-hexane layer was absorbed and determined by gas chromatography mass spectrometry(GC-MS),and the salicylic acid internal standard method was used for quantitative determination.Results The correlation coefficients(r)of the five preservatives were all greater than 0.99 in the range of 1.0μg/ml-50μg/ml.The limit of detection was within 0.33 mg/kg-1.0 mg/kg,and the limit of quantification was within 1.09 mg/kg-3.0 mg/kg.The average recoveries were within 83.6%-109.19%,and the relative standard deviations(RSD)were within 1.74%-8.77%(n=6).Conclusion This method has low sample con⁃sumption,high sensitivity,simple and fast operation,and is suitable for the simultaneous determination of multiple preservatives in pastry.

关 键 词：糕点 防腐剂 衍生 气相色谱-质谱联用法 

分 类 号：O657[理学—分析化学]