悬浮液进样-石墨炉原子吸收光谱法测定巴戟天中痕量铅和镉
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摘要
取经烘干粉碎并通过0.074mm网筛的巴戟天样品0.050 0g,加入琼脂溶液10.0mL(其中含磷酸二氢铵0.1g,作为基体改进剂),超声振荡5min,制成样品的悬浮液,直接进样,采用石墨炉原子吸收光谱法测定其中铅和镉的含量。设置铅和镉的灰化温度分别为850℃和800℃。结果表明:铅和镉的质量浓度在一定范围内与其吸光度呈线性关系,铅和镉的检出限(3s×V/b)分别为2.17×10-9 mg和3.4×10-10 mg。按照标准加入法进行加标回收试验,铅和镉的回收率分别在98.8%～103%和98.3%～104%之间。精密度试验表明铅和镉的测定值的相对标准偏差(n=7)分别为2.7%和1.2%。
0.050 0 g of the dried and powdered morinda officinalis sample(passed through 0.074 mm sample sieve)was taken and dispended in 10.0 mL of agar solution(containing 0.1 g of NH4 H2 PO4 as matrix modifier)with an ultrasonotor for 5 min,to make a suspension of the sample which was introduced into the instrument for GF-AAS determination of lead and cadmium.Ashing temperatures for lead and cadmium were set at 850 ℃ and800℃,respectively.As shown by the results,linear relationships between values of absorbance and mass concentration of lead and cadmium were found in definite ranges,with detection limits(3 s×V/b)of 2.17×10-9 mg and 3.4×10-10 mg respectively.Test for recovery was made by standard addition method,giving results in the range of 98.8%-103% and 98.3%-104%,respectively.Values of RSDs(n=7)were found 2.7%(for Pb)and 1.2%(for Cd).
0.050 0 g of the dried and powdered morinda officinalis sample(passed through 0.074 mm sample sieve)was taken and dispended in 10.0 mL of agar solution(containing 0.1 g of NH4 H2 PO4 as matrix modifier)with an ultrasonotor for 5 min,to make a suspension of the sample which was introduced into the instrument for GF-AAS determination of lead and cadmium.Ashing temperatures for lead and cadmium were set at 850 ℃ and800℃,respectively.As shown by the results,linear relationships between values of absorbance and mass concentration of lead and cadmium were found in definite ranges,with detection limits(3 s×V/b)of 2.17×10-9 mg and 3.4×10-10 mg respectively.Test for recovery was made by standard addition method,giving results in the range of 98.8%-103% and 98.3%-104%,respectively.Values of RSDs(n=7)were found 2.7%(for Pb)and 1.2%(for Cd).
引文
[1]卢化柱.《随园食单》中的药物—药食同源的个案研究[D].成都:成都中医药大学,2013.
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[6]苏耀东,刘宏,王伟锋,等.超声搅拌悬浮液进样石墨炉原子吸收测定海洋沉积物中的痕量镉[J].理化检验-化学分册,2000,36(11):506-507.
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[10] PENG Y,GUO W,ZHANG P,et al.Heat-assisted slurry sampling GFAAS method for determination of lead in food standard reference materials[J].Journal of Food Composition and Analysis,2015,42:78-83.
[11]邓世林,李新凤,邓富良.固体悬浮液进样石墨炉原子吸收法测定茶叶中的微量镉[J].食品科学,2004,25(2):141-143.
[12]陈江,周李,姚恩亲.悬浮液进样石墨炉原子吸收法测定茶叶中镍含量[J].光散射学报,2011,23(1):70-74.
[13]张锂,韩国才.悬浮液进样-石墨炉原子吸收光谱法测定生物样品中微量铬[J].理化检验-化学分册,2008,44(4):361-363.
[14]张换平,杜慧,王书红,等.悬浮液进样-石墨炉原子吸收光谱法测定中药中铜和铅的溶出率[J].理化检验-化学分册,2018,54(3):360-362.
[15]周陶鸿,林津,彭青枝,等.悬浮液进样石墨炉原子吸收光谱法测定乳粉中痕量铬[J].食品安全质量检测学报,2015,6(4):1478-1482.
[16] GB 5009.12-2017食品安全国家标准食品中铅的测定[S].
[17] GB 5009.15-2014食品安全国家标准食品中镉的测定[S].
[18] WM/T 2-2004药用植物及制剂外经贸行业标准[S].
[2]罗盛旭,李金英,胡广林,等.巴戟天中微量元素的形态分析[J].时珍国医国药,2008,19(12):3016-3019.
[3]丁平,刘硕,刘瑾,等.巴戟天中微量元素与土壤中矿质元素的相关性分析[J].华西药学杂志,2010,25(6):727-729.
[4]陈荣溢,宋婷婷.广东植物类中药材出口现状及对策初探[J].广东农业科学,2007,39(2):105-106.
[5]孙汉文,温晓华,梁淑轩.悬浮体进样-基体改进效应石墨炉原子吸收光谱法直接测定土壤中的铅和镉[J].光谱学与光谱分析,2006,26(5):950-954.
[6]苏耀东,刘宏,王伟锋,等.超声搅拌悬浮液进样石墨炉原子吸收测定海洋沉积物中的痕量镉[J].理化检验-化学分册,2000,36(11):506-507.
[7] TINAS H,OZBEK N,AKMAN S.Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2018,140:73-75.
[8] AMORIM F A C,COSTA V C,GUEDES W N,et al.Multivariate optimization of method of slurry sampling for determination of iron and zinc in starch samples by flame atomic absorption spectrometry[J].Food Analytical Methods,2016,9(6):1719-1725.
[9] DOS SANTOS W N L, CAVALCANTEDD,MACEDO S M,et al.Slurry sampling and HG AFS for the determination of total arsenic in rice samples[J].Food Analytical Methods,2013,6(4):1128-1132.
[10] PENG Y,GUO W,ZHANG P,et al.Heat-assisted slurry sampling GFAAS method for determination of lead in food standard reference materials[J].Journal of Food Composition and Analysis,2015,42:78-83.
[11]邓世林,李新凤,邓富良.固体悬浮液进样石墨炉原子吸收法测定茶叶中的微量镉[J].食品科学,2004,25(2):141-143.
[12]陈江,周李,姚恩亲.悬浮液进样石墨炉原子吸收法测定茶叶中镍含量[J].光散射学报,2011,23(1):70-74.
[13]张锂,韩国才.悬浮液进样-石墨炉原子吸收光谱法测定生物样品中微量铬[J].理化检验-化学分册,2008,44(4):361-363.
[14]张换平,杜慧,王书红,等.悬浮液进样-石墨炉原子吸收光谱法测定中药中铜和铅的溶出率[J].理化检验-化学分册,2018,54(3):360-362.
[15]周陶鸿,林津,彭青枝,等.悬浮液进样石墨炉原子吸收光谱法测定乳粉中痕量铬[J].食品安全质量检测学报,2015,6(4):1478-1482.
[16] GB 5009.12-2017食品安全国家标准食品中铅的测定[S].
[17] GB 5009.15-2014食品安全国家标准食品中镉的测定[S].
[18] WM/T 2-2004药用植物及制剂外经贸行业标准[S].