自动顶空毛细柱气相色谱内标法测定食用植物油六号溶剂残留量
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摘要
目的建立顶空-毛细柱气相色谱内标法测定食用植物油中六号溶剂残留量的检测方法。方法以氮气为载气,采用气液顶空气相色谱法,试样在70℃,平衡30 min后经HP-5毛细柱分离,FID检测,正庚烷内标法定量,测定试样中六号溶剂残留量含量。结果六号溶剂含量在10 mg/kg～200 mg/kg内线性关系良好,相关系数均≥0.999 80,方法检出限为0.70 mg/kg。配制20.0 mg/kg、50.0 mg/kg、200.0 mg/kg 3个不同浓度加标样品并平行进样6次,其平均回收率为95.1%～103.0%,相对标准偏差为3.1%～4.4%。结论本方法操作简单,自动化程度高,分离效果好,灵敏度高,重现性好,在较宽的线性范围内有良好的准确度和精密度,结果准确可靠,可应用于日常工作中食用植物油中六号溶剂残留量的检测分析。
Objective To establish an auto headspace capillary gas chromatography method with internal standard for the determination of No.6 solvent residual in edible vegetable oil. Methods Based on the auto headspace sampling method, N_2 was adopted as the carrier gas. The samples were separated by the HP-5 capillary column after balanced at 70 ℃ for 30 minutes, and then monitored by the detector of FID and quantified by the n-heptane internal standard. Results It showed the good linearity was obtained within 10 mg/kg-200 mg/kg, with the correlation coefficients all above 0.999 8. The detection limits of the method was 0.70 mg/kg. The recoveries of 20.0 mg/kg, 50.0 mg/kg and 200.0 mg/kg ranged from 95.1% to 103.0%, with RSD of 3.1%-4.4%. Conclusion This method is simple, automatic, accurate and precise. It is suitable for the determination of No.6 solvent residual in edible vegetable oil.
Objective To establish an auto headspace capillary gas chromatography method with internal standard for the determination of No.6 solvent residual in edible vegetable oil. Methods Based on the auto headspace sampling method, N_2 was adopted as the carrier gas. The samples were separated by the HP-5 capillary column after balanced at 70 ℃ for 30 minutes, and then monitored by the detector of FID and quantified by the n-heptane internal standard. Results It showed the good linearity was obtained within 10 mg/kg-200 mg/kg, with the correlation coefficients all above 0.999 8. The detection limits of the method was 0.70 mg/kg. The recoveries of 20.0 mg/kg, 50.0 mg/kg and 200.0 mg/kg ranged from 95.1% to 103.0%, with RSD of 3.1%-4.4%. Conclusion This method is simple, automatic, accurate and precise. It is suitable for the determination of No.6 solvent residual in edible vegetable oil.
引文
[1] 章晴,陈士恒,高丁,等.顶空-气相色谱法测定食用植物油中溶剂残留的方法研究[J].分析测试技术与仪器,2015,21(4):225-230.
[2] 秦德萍,毛庆,韩燕,等.顶空-气相色谱法测定食用植物油中溶剂残留量[J].食品与药品,2017,19(5):347-350.
[3] 金俊,张友峰,陈金平,等.几种常见食用植物油溶剂残留量检测和残留溶剂组分分析[J].粮食和油脂,2016,29(12):75-78.
[4] 王乐华.食用植物油浸出溶剂评价及溶剂残留检测方法研究[D].苏州:苏州大学,2013.
[5] 孙黎黎,邵守峰.食用植物油中残留溶剂测定方法的改进[J].中国卫生检验杂志,2005,15(3):360-360.
[6] 赵金利,宋安华,陈慧琴,等.顶空气相色谱法测定香型食用油中六号溶剂的残留量[J].食品安全质量检测学报,2017,8(4):1274-1279.
[7] 林飞,罗飞亚.正己烷的毒理学研究现状及风险评估[J].中国药事,2013,27(5):525-529.
[8] 王磊,肖聪伟,肖微.应用程序升温毛细管气相色谱法检测食用植物油中溶剂残留研究[J].质量探索,2013(11):48-49.
[9] 曾文锦.顶空气相色谱毛细管柱法测定浸出食用油溶剂残留量色谱条件的探讨[J].化工管理,2015(21):49-50.
[10] 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.
[11] 张海.毛细管柱气相色谱法测定食用油中溶剂残留[J].品牌与标准化,2015(4):50-51.
[12] 徐陆妹.食用植物油中残留溶剂测定的方法研究[J].中国卫生检验杂志,2009,19(4):775-805.
[13] 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.
[14] 黄韬睿,王鑫.毛细管气相色谱法测定市售食用油中残留溶剂的研究[J].生命科学仪器,2012,10(4):45-46.
[15] 邢峰,郑军科,金绍强,等.顶空气相色谱法检测食用植物油中溶剂的残留[J].浙江农业科学,2015,56(7):1078-1083.
[16] 中华人民共和国国家质量监督检验检疫总局.GB 16629—2008植物油抽提溶剂[S].北京:中国标准出版社,2008.
[2] 秦德萍,毛庆,韩燕,等.顶空-气相色谱法测定食用植物油中溶剂残留量[J].食品与药品,2017,19(5):347-350.
[3] 金俊,张友峰,陈金平,等.几种常见食用植物油溶剂残留量检测和残留溶剂组分分析[J].粮食和油脂,2016,29(12):75-78.
[4] 王乐华.食用植物油浸出溶剂评价及溶剂残留检测方法研究[D].苏州:苏州大学,2013.
[5] 孙黎黎,邵守峰.食用植物油中残留溶剂测定方法的改进[J].中国卫生检验杂志,2005,15(3):360-360.
[6] 赵金利,宋安华,陈慧琴,等.顶空气相色谱法测定香型食用油中六号溶剂的残留量[J].食品安全质量检测学报,2017,8(4):1274-1279.
[7] 林飞,罗飞亚.正己烷的毒理学研究现状及风险评估[J].中国药事,2013,27(5):525-529.
[8] 王磊,肖聪伟,肖微.应用程序升温毛细管气相色谱法检测食用植物油中溶剂残留研究[J].质量探索,2013(11):48-49.
[9] 曾文锦.顶空气相色谱毛细管柱法测定浸出食用油溶剂残留量色谱条件的探讨[J].化工管理,2015(21):49-50.
[10] 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.
[11] 张海.毛细管柱气相色谱法测定食用油中溶剂残留[J].品牌与标准化,2015(4):50-51.
[12] 徐陆妹.食用植物油中残留溶剂测定的方法研究[J].中国卫生检验杂志,2009,19(4):775-805.
[13] 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.
[14] 黄韬睿,王鑫.毛细管气相色谱法测定市售食用油中残留溶剂的研究[J].生命科学仪器,2012,10(4):45-46.
[15] 邢峰,郑军科,金绍强,等.顶空气相色谱法检测食用植物油中溶剂的残留[J].浙江农业科学,2015,56(7):1078-1083.
[16] 中华人民共和国国家质量监督检验检疫总局.GB 16629—2008植物油抽提溶剂[S].北京:中国标准出版社,2008.