石墨炉原子吸收光谱法测定高盐食品中的微量铅
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摘要
建立石墨炉原子吸收光谱法测定高盐食品中微量铅的含量。试样经硝酸消解,恒温加热赶酸后,采用Ag离子小柱洗脱除盐。石墨炉加热程序:干燥150℃,持续30 s;干燥2 140℃,持续20 s;灰化550℃,持续20 s;原子化温度为2 000℃,持续4 s。光电倍增管电压为506 V,灯电流为6 mA,波长为283.3 nm,狭缝宽度为0.4 nm,时间常数为0.1 s,采用塞曼效应背景校正。食品含盐量在20%以内对铅的测定无显著影响。铅的质量浓度在0～30ng/mL范围内与吸光度呈良好的线性关系,线性相关系数为0.999 8,方法检出限为0.005 mg/kg。测定结果的相对标准偏差为1.58%～2.16%(n=7),样品加标回收率为82.40%～107.89%。该方法灵敏度高,结果准确、可靠,适用于高盐食品中微量铅的检测。
A method for the determination of trace lead in high salt food by graphite furnace atomic absorption spectrometry was established. The sample was digested by nitric acid and heated at constant temperature to expel acid. The salt was removed by Agion extraction column. The heating procedure of graphite furnace was optimized as: dried at 150℃for 30 seconds; dried at 2 140℃ for 20 seconds; ashed at 550℃ for 20 seconds; atomization at 2 000℃ for 4 seconds. The voltage of the photomultiplier was 506 V, the lamp current was 6 mA, the wavelength was 283.3 nm, the slit width was 0.4 nm, and the time constant was 0.1 s. Zeeman effect background correction was used. The salt content of food within 20%had no effect on the determination of lead. The mass concentration of lead had a good linear relationship with absorbance in the range of 0–30 ng/mL, the linear correlation coef?cient was 0.999 8, and the detection limit was 0.005 mg/kg. The relative standard deviations were 1.58%–2.16%(n=7), and the recoveries were 82.40%–107.89%. The method is sensitive,accurate and reliable, and it is suitable for the determination of trace lead in high salt food.
A method for the determination of trace lead in high salt food by graphite furnace atomic absorption spectrometry was established. The sample was digested by nitric acid and heated at constant temperature to expel acid. The salt was removed by Agion extraction column. The heating procedure of graphite furnace was optimized as: dried at 150℃for 30 seconds; dried at 2 140℃ for 20 seconds; ashed at 550℃ for 20 seconds; atomization at 2 000℃ for 4 seconds. The voltage of the photomultiplier was 506 V, the lamp current was 6 mA, the wavelength was 283.3 nm, the slit width was 0.4 nm, and the time constant was 0.1 s. Zeeman effect background correction was used. The salt content of food within 20%had no effect on the determination of lead. The mass concentration of lead had a good linear relationship with absorbance in the range of 0–30 ng/mL, the linear correlation coef?cient was 0.999 8, and the detection limit was 0.005 mg/kg. The relative standard deviations were 1.58%–2.16%(n=7), and the recoveries were 82.40%–107.89%. The method is sensitive,accurate and reliable, and it is suitable for the determination of trace lead in high salt food.
引文
[1]GB 5009.12-2017食品中铅的测定[S].
[2]王玲,郝晓宏,王彩云,等.石墨炉原子吸收光谱法测定食品中铅含量的测定不确定度分析[J].实用医学杂志,2011,18(4):387.
[3]刘双,周静.石墨炉原子吸收光谱法测定食品中铅的方法研究[J].公共卫生与预防医学,2007,18(10):71-72.
[4]冯银凤,黄诚,周日东,等.基体改进剂在石墨炉原子吸收光谱法测定食品中铅含量的讨论[J].中国卫生检验杂志,2005,15(4):450-472.
[5]任婷,赵丽娇,曹珺,等.高分辨率连续光谱石墨炉原子吸收光谱法测定食品中铅、镉和铬含量[J].光谱学与光谱分析,2012,32(9):2 566-2 571.
[6]王丽娟,胡军妹,严正,等.石墨炉原子吸收光谱法测定食品中铅和镉的基体改进剂研究[J].中外健康文摘,2011,45(8):58-60.
[7]杨佳佳,孙海波,杨彦丽,等.高盐食品中铅的测定方法的研究进展[J].食品安全质量检测学报,2016,7(4):1 462-1 465.
[8]赵志远,贺国庆,李佳颖.高盐食品中铅含量检测方法概述[J].食品与发酵工业,2012,38(8):146-149.
[9]宋美美,冯志强,郭秋兰,等.石墨炉原子吸收光谱法测定高盐食品中重金属的研究进展[J].食品与发酵科技,2015,51(4):92-95.
[10]常松.标准加入-洗脱法测定高盐食品中铅含量[J].安徽农学通报(下半月刊),2011,17(18):64-65.
[11]时二静,马迎辉,司静静,等.基替改进剂用于GFAAS测定高盐食品中铅的研究[J].河南科技,2016(13):128-131.
[12]姜杰,林凯,张慧敏,等.高盐食品中铅的石墨炉原子吸收光谱测定法[J].职业与健康,2012,28(2):187-189.
[13]何健,冯民,朱臻怡,等.Chelex-100树脂对铅、镉、钠的吸附性能及其应用于原子吸收光谱法测定高盐食品中的铅、镉含量[J].理化检验(化学分册),2013,49(2):170-173.
[14]陈林军.石墨炉原子吸收光谱法测定含盐食品中的铅[J].理化检验(化学分册),2012,48(2):169-170.
[15]李晓红,丁琳,徐榕蔓,等.溶剂萃取-石墨炉原子吸收法测定高盐份酱油中的铅[J].西北农业学报,2009,18(1):255-257.
[16]胡曙光,苏祖俭,蔡文华,等.石墨炉原子吸收光谱法测定含盐食品中的铅及其干扰消除的研究[J].中国食品卫生杂志,2015,27(4):394-398.
[17]GB/T8170-2008数值修约规则与极限数值的表示和判定[S].
[2]王玲,郝晓宏,王彩云,等.石墨炉原子吸收光谱法测定食品中铅含量的测定不确定度分析[J].实用医学杂志,2011,18(4):387.
[3]刘双,周静.石墨炉原子吸收光谱法测定食品中铅的方法研究[J].公共卫生与预防医学,2007,18(10):71-72.
[4]冯银凤,黄诚,周日东,等.基体改进剂在石墨炉原子吸收光谱法测定食品中铅含量的讨论[J].中国卫生检验杂志,2005,15(4):450-472.
[5]任婷,赵丽娇,曹珺,等.高分辨率连续光谱石墨炉原子吸收光谱法测定食品中铅、镉和铬含量[J].光谱学与光谱分析,2012,32(9):2 566-2 571.
[6]王丽娟,胡军妹,严正,等.石墨炉原子吸收光谱法测定食品中铅和镉的基体改进剂研究[J].中外健康文摘,2011,45(8):58-60.
[7]杨佳佳,孙海波,杨彦丽,等.高盐食品中铅的测定方法的研究进展[J].食品安全质量检测学报,2016,7(4):1 462-1 465.
[8]赵志远,贺国庆,李佳颖.高盐食品中铅含量检测方法概述[J].食品与发酵工业,2012,38(8):146-149.
[9]宋美美,冯志强,郭秋兰,等.石墨炉原子吸收光谱法测定高盐食品中重金属的研究进展[J].食品与发酵科技,2015,51(4):92-95.
[10]常松.标准加入-洗脱法测定高盐食品中铅含量[J].安徽农学通报(下半月刊),2011,17(18):64-65.
[11]时二静,马迎辉,司静静,等.基替改进剂用于GFAAS测定高盐食品中铅的研究[J].河南科技,2016(13):128-131.
[12]姜杰,林凯,张慧敏,等.高盐食品中铅的石墨炉原子吸收光谱测定法[J].职业与健康,2012,28(2):187-189.
[13]何健,冯民,朱臻怡,等.Chelex-100树脂对铅、镉、钠的吸附性能及其应用于原子吸收光谱法测定高盐食品中的铅、镉含量[J].理化检验(化学分册),2013,49(2):170-173.
[14]陈林军.石墨炉原子吸收光谱法测定含盐食品中的铅[J].理化检验(化学分册),2012,48(2):169-170.
[15]李晓红,丁琳,徐榕蔓,等.溶剂萃取-石墨炉原子吸收法测定高盐份酱油中的铅[J].西北农业学报,2009,18(1):255-257.
[16]胡曙光,苏祖俭,蔡文华,等.石墨炉原子吸收光谱法测定含盐食品中的铅及其干扰消除的研究[J].中国食品卫生杂志,2015,27(4):394-398.
[17]GB/T8170-2008数值修约规则与极限数值的表示和判定[S].