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作 者:韩婷婷[1,2] 崔鹤[2] 段小娟 宋田[4] 姬泓巍[1] 李慧新[2] 蔡峰[2] 朱倩林[1]
机构地区:[1]中国海洋大学化学化工学院,山东青岛266100 [2]山东出入境检验检疫局检验检疫技术中心,山东青岛266002 [3]青岛出入境检验检疫局,山东青岛266001 [4]燕山大学理学院,河北秦皇岛066004
出 处:《食品科学》2016年第14期169-173,共5页Food Science
基 金:国家重大科学仪器设备开发专项(2012YQ090229)
摘 要:建立离子色谱等度分离测定碳酸盐及磷酸盐中F^-、Cl^-、SO_4^(2-)、NO_3^(-4)种无机阴离子的方法,碳酸盐试样用20 mmol/L氢氧化钠溶液溶解,加磷酸中和至p H 4.5~5.5;磷酸盐试样直接用20 mmol/L氢氧化钠溶液溶解。色谱柱采用AS11-HC分离柱,流动相20 mmol/L氢氧化钠溶液,流速1.0 m L/min。结果表明:F^-、Cl^-、SO_4^(2-)、NO_3^(-4)种阴离子质量浓度与峰面积呈良好线性关系(r=0.999 2~0.999 9),检出限分别为2.0、2.0、2.5、2.5 mg/kg,在低、中、高3个加标水平下的平均回收率为80%~109.88%,相对标准偏差为0.85%~4.67%(n=6)。该方法准确、简便、灵敏、通用、重复性好,可用于碳酸盐及磷酸盐中4种阴离子的实际检测。An analytical method using ion chromatography with isocratic elution was developed for the determination of four inorganic anions(F^-, Cl^-, SO_4^(2-) and NO_3^-) in carbonates and phosphates. Carbonate samples were dissolved in 20 mmol/L sodium hydroxide solution and then neutralized to p H between 4.5 and 5.5 with phosphoric acid. Phosphate samples were dissolved with 20 mmol/L sodium hydroxide solution directly and then separated on an AS11-HC column with 20 mmol/L sodium hydroxide solution as the mobile phase at 1.0 m L/min flow rate. The results indicated that the calibration curves showed good linear relationship for 4 inorganic anions(r = 0.999 2–0.999 9). The limits of detection(LODs) for F^-, Cl^-, SO_4^(2-) and NO_3^- were 2.0, 2.0, 2.5 and 2.5 mg/kg respectively. The mean recoveries at three spiked concentration levels(low, middle, and high) were 80%–109.88%, and the relative standard derivations(RSDs) were 0.85%–4.67%(n = 6). The proposed method is reliable, simple, convenient, sensitive, universal and reproducible, and can be applied in the rapid determination of 4 anions in carbonates and phosphates.
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