阴离子交换离子色谱法测定卷烟纸中乙酸盐、磷酸盐和柠檬酸盐含量  

Anion Exchange-Ion Chromatographic Determination of Acetate Phosphate and Citrate in Cigarette Paper

作　　者：王荔[1] 宋国新[1] 邓春晖[2] 

机构地区：[1]复旦大学分析测试中心,上海200433 [2]复旦大学化学系,上海200433

出　　处：《理化检验（化学分册）》2009年第7期815-817,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：用水对卷烟纸中乙酸根、磷酸根及柠檬酸根3种阴离子进行超声提取，所得提取液经0．45μm滤膜过滤后上机进行离子色谱分析。采用IONPAC AS15分离柱和IONPAC AG15保护柱，并采用70mmol·L^-1氢氧化钠溶液作为淋洗液进行梯度淋洗，从而实现上述3种阴离子的分离。采用电导检测进行定量，3种阴离子的峰面积的积分值与其相应浓度之间的线性范围为：0．2～50mg·L^-1（乙酸根），0．5～50mg·L^-1（磷酸根）和0．5～100mg·L^-1（柠檬酸根）。方法的检出限（3S／N）依次为0．2，0．4，0．5mg·L^-1。取含有乙酸根5mg·L^-1和磷酸根及柠檬酸根各10mg·L^-1的混合标准溶液按方法进行分析，进样7次，根据所得测定值求算其相对标准偏差依次为1．2％，1．8％，1.3％。在3种不同浓度水平上，用标准加入法作回收试验，所得结果为96．6％～106．5％（乙酸根），94．5％～107．8％（磷酸根），88．3％-1003．6％（柠檬酸根）。The objective anions （acetate, phosphate and citrate） were extracted ultrasonically from cigarette paper with water, and the extract obtained was filtered with 0. 45μm filtering membrane, and introduced into the instrument for IC determination. IONPAC AS15 column was used for separation, and the IONPAC AG15 was used as guard column. Seventy 70 mmol · L^-1 NaOH solution was used as eluent for gradient elution. Conductivity detection was adopted in the determination. Linear relationships between values of integrals of peak area and concentration of the 3 anions were obtained in the ranges of 0. 2-50 mg · L^-1 （for acetate）, 0. 5-50 mg · L^-1 （for phosphate） and 0. 5-100 mg · L^-1 （for citrate）, with detection limits （3S/N） of 0. 2, 0. 4, 0. 5 mg · L^-1 respectively. Precision of the method was tested by analyzing a mixed standard solution containing 5 mg · L^-1 of acetate and 10 mg · L^-1 each of phosphate and citrate, values of RSD＇s （n=7） obtained were 1.2%, 1.8% and 1.3% respectively. Recovery was tested at 3 different concentration levels, and the results obtained were in the ranges of 96.6%-106.5% （for acetate）, 94. 5%-107. 8% （for phosphate） and 88. 3%-103.6% （for citrate）.

关 键 词：离子色谱法 乙酸根 磷酸根 柠檬酸根 卷烟纸 

分 类 号：O652.63[理学—分析化学]