HS-GC-FID法测定豆粕中6种溶剂残留
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摘要
建立了顶空-气相色谱-氢火焰离子化检测法(HS-GC-FID)测定豆粕中6种烷烃类残留溶剂的新方法。豆粕样品经80℃振荡平衡30min后即可进样分析,采用Rxi-5Sil MS毛细管柱分离,FID测定,外标法定量。结果表明,6种目标分析物在0.2～10.0mg/kg间均呈现良好线性关系,相关系数(R2)大于0.990,方法检测限(LOD)0.075mg/kg,定量限(LOQ)0.2mg/kg,平均加标回收率95.3%～106.3%,相对标准偏差(RSD)小于8.3%。该方法操作简单且灵敏度高,可满足豆粕中残留溶剂的日常检测需要。
The samples were oscillated for 30 min at 80℃prior to sample injection.The separation was performed on a Rxi-5 Sil MS column.The six analytes were determined by FID,quantified by using external standards method.Linear range of 0.2 —10.0 mg/kg were obtained with linear correlation coefficient(R2)over than 0.990.The LOD and LOQ values were 0.075 mg/kg and 0.2 mg/kg respectively.The average recoveries were between 95.3% and 106.3% with relative standard deviations(RSD)less than8.3%.This method is simple,sensitive,and suitable for the routine analysis of residual solvents in soybean meal.
The samples were oscillated for 30 min at 80℃prior to sample injection.The separation was performed on a Rxi-5 Sil MS column.The six analytes were determined by FID,quantified by using external standards method.Linear range of 0.2 —10.0 mg/kg were obtained with linear correlation coefficient(R2)over than 0.990.The LOD and LOQ values were 0.075 mg/kg and 0.2 mg/kg respectively.The average recoveries were between 95.3% and 106.3% with relative standard deviations(RSD)less than8.3%.This method is simple,sensitive,and suitable for the routine analysis of residual solvents in soybean meal.
引文
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[3]汪文忠.豆粕在鱼饲料中的应用[J].齐鲁渔业,2015,32(7):37-38.
[4]吴业阳,孙瑞健,米海峰,等.生物发酵饲料现状及在水产养殖上应用[J].中国饲料,2018(13):60-63.
[5]宋向荣,赵娜,周志洋,等.职业性正己烷接触工人外周血红细胞血影蛋白表达的研究[J].中国辐射卫生,2017,26(4):482-485.
[6]张维森.烃类有机溶剂职业病危害的预防与控制[J].中国工业医学杂志,2008,21(2):129-131.
[7]蓝芳,谢丽琪,杨左军,等.顶空固相微萃取-气相色谱法测定油脂中浸出油溶剂残留的方法研究[J].分析试验室,2004,23(4):70-72.
[8]马君刚,丁春瑞,菅丽君.顶空气相色谱法测定植物油中的溶剂残留量[J].食品工程,2013(4):50-52.
[9]王永芳,葛含光,王利强,等.顶空气相色谱法快速测定食用植物油中有机溶剂残留量的研究[J].食品安全质量检测学报,2015,6(2):432-435.
[10]辛凤鲜.气相色谱测定豆粕残溶条件的研究[J].中国油脂,2003,28(4):58-59.
[11]董晓丽,孙娟,张妍,等.顶空气相色谱法测定豆粕中残留溶剂研究[J].中国油料作物学报,2013,35(4):436-440.
[12]马灵飞,周围,张雅珩,等.顶空-气相色谱法测定葵花籽粕中六号溶剂残留量[J].食品安全质量检测学报,2015,6(11):4422-4427.
[13]马建华.顶空气相色谱法测定食品中甜蜜素含量[J].中国环境管理干部学院学报,2005,15(1):38-41.
[14]徐爱军,李丹.大豆粕溶剂残留测定方法研究[J].安徽农业科学,2018,46(1):178-180.