IC Determination of Sulfite in Konjak Refined Powder and Shrimp
摘 要
魔芋精粉和虾样品经水蒸气蒸馏除去杂质的干扰,在密闭容器中对样品进行酸化,在氮气流的保护下蒸馏,用甲醛溶液吸收释放出的二氧化硫,提出了离子色谱法测定样品中亚硫酸盐含量的方法。以IonPac AS9-HC色谱柱,以8 mmol·L-1碳酸钠-2.5 mmol·L-1氢氧化钠溶液为淋洗液等度洗脱,用电导检测器测定。亚硫酸盐的质量浓度在6.0 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为4.0 mg·kg-1。方法用于魔芋精粉和虾样品分析,回收率在88.1%~98.3%之间,测定值的相对标准偏差(n=8)在1.4%~6.6%之间。
Abstract
Samples of konjak refined powder and shrimp were distilled by steam distillation method to eliminate the interference of impurity, and acidified in closed vessel. The SO2 was evolved under nitrogen atmosphere and absorbed in formaldehyde solution. The content of sulfite in absorption solution was determined by IC. IonPac AS9-HC chromatographic column was used as ion exchange column, and a mixture of 8 mmol·L-1 Na2CO3 and 2.5 mmol·L-1 NaOH was used as eluent. Linear relationship between values of peak area and mass concentration of sulfite was obtained in the range within 6.0 mg·L-1, with detection limit (3S/N) of the method of 4.0 mg·kg-1. The proposed method has been used in the analysis of the samples of konjak refined powder and shrimp, giving values of recovery and RSD′s (n=8) in the ranges of 88.1%-98.3% and 1.4%-6.6% respectively.
中图分类号 O657.72
所属栏目 工作简报
基金项目 国家认证认可监督委员会资助行业标准项目(2007B146)
收稿日期 2011/2/11
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备注黄惠玲(1969-),女,海南海口人,高级工程师,主要研究方向为食品残留分析。
引用该论文: HUANG Hui-ling,WANG Yu-jian,XU Li,JI Shao-fan,HUANG Hai-min,LIN Zheng-feng,CAI Wei-kai. IC Determination of Sulfite in Konjak Refined Powder and Shrimp[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(3): 339~341
黄惠玲,王玉健,徐莉,纪少凡,黄海民,林正锋,蔡伟凯. 离子色谱法测定魔芋精粉、虾中亚硫酸盐[J]. 理化检验-化学分册, 2012, 48(3): 339~341
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参考文献
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【2】高鹤娟.食品卫生检验方法[M].北京:中国轻工业出版社, 1992:35-39.
【3】GB 2760-2000食品添加剂使用卫生标准[S].
【4】GB/T 5009.34-2003食品中亚硫酸盐的测定方法[S].
【5】SN/T 0857-2000进出口啤酒中二氧化硫的检验方法[S].
【6】SN/T 0230.(1/2)-1993出口脱水蔬菜(大蒜制品)检验规程[S].
【7】ISO 5522-1981水果、蔬菜及其制品——二氧化硫总量的测定[S].
【8】KIM H J. Determination of sulfites in foods and beverages by ion exclusion chromatography with electrochemical detection: collaborative study[J]. J Assoc off Anal Chem, 1990,73(2):216-223.
【9】刘喆,刘克纳,宋强,等.离子排斥色谱法-脉冲安培检测器对食品中亚硫酸及其盐的分析与检测[J].食品与发酵工业, 1997,23(4):19-20.
【10】ARANTZA A A, PENA-EGIDO M J. Improved method for determination of sulfites in shrimp[J]. Journal of AOAC International, 1993,76(3):565-571.
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