电感耦合等离子体质谱法快速测定胶囊中铬的含量
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摘要
目的采用动态反应池-电感耦合等离子体质谱技术,建立快速测定胶囊中铬的分析方法。方法预消化-微波消解处理胶囊样品,采用动态反应池模式消除干扰,选择反应气NH3,流速为0.6ml/min,Rpq为0.55,将可能干扰铬测定的40Ar12C+、37Cl16O+等离子强度值降低了大约2个数量级。结果铬元素测定标准曲线的线性相关系数为0.9996,以称样量0.5g计,方法检出限为0.03mg/kg,样品加标回收率为86.5%～107.8%,相对标准偏差<5%。结论该方法精密度好、准确性好,适用于胶囊中铬含量的快速、准确测定。
Objective To establish the method which determined the content of chromium(Cr) in capsule by inductively coupled plasma-mass spectrometry.Methods Pre-digestion-microwave digestion procedures were applied to extract Cr from the capsules.The potentially interfering 40Ar12C+ and 37Cl16O+ at the chromium masses m/z 52 and 53 were reduced in intensity by approximately 2 orders of magnitude by using 0.6 ml/min NH3 as reactive cell gas in the dynamic reaction cell(DRC) while a Rpq value of 0.55 was used.Results The correlation coefficient(r) of standard curve was 0.9996,and the detection limit of the method was 0.03mg/kg,and the average recoveries for all determinations ranged from 86.5% to 107.8% with the related standard deviation below 5%.Conclusion The method,which is of good precision and accuracy,is applicable to rapid and accurate determination of chromium content in capsule.
Objective To establish the method which determined the content of chromium(Cr) in capsule by inductively coupled plasma-mass spectrometry.Methods Pre-digestion-microwave digestion procedures were applied to extract Cr from the capsules.The potentially interfering 40Ar12C+ and 37Cl16O+ at the chromium masses m/z 52 and 53 were reduced in intensity by approximately 2 orders of magnitude by using 0.6 ml/min NH3 as reactive cell gas in the dynamic reaction cell(DRC) while a Rpq value of 0.55 was used.Results The correlation coefficient(r) of standard curve was 0.9996,and the detection limit of the method was 0.03mg/kg,and the average recoveries for all determinations ranged from 86.5% to 107.8% with the related standard deviation below 5%.Conclusion The method,which is of good precision and accuracy,is applicable to rapid and accurate determination of chromium content in capsule.
引文
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2廖自基.微量元素的环境化学及生物效应[M].北京:中国环境科学出版社,1992:288-291.
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4 GOMEZ V,CALLAO M P.Chromium determinationand speciation since 2000[J].Trends Anal Chem,2006,25(10):1006-1015.
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6陈超,陈瑜,俞辉.微波消解石墨炉原子吸收光谱法测定胶囊和片剂用明胶中铬含量[J].分析化学,2006,34(12):1820.
7石岩,肖新月,石上梅,等.微波消解-石墨炉原子吸收法测定阿胶中铬含量[J].药物分析杂志,2011,31(8):1527.
8 European Pharmacopoeia Commission.EuropeanPharmacopoeia 7thEdition[M].European Directorate forthe Quality of Medicines,2012:707-709.
9国家药典委员会.中国药典第二部[M].北京:中国医药科技出版社,2010:1204.
10中华人民共和国卫生部.GB/T5009.123—2003食品中铬的测定[S].北京:中国标准出版社,2003.
11丁春光,朱醇,刘德晔,等.电感耦合等离子体质谱方法检测全血中30种金属及类金属元素[J].中华预防医学杂志,2012,46(8):745-749.
12王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社,2005:80-95.
13 SUN Y C,LIN C Y,WU S F,et al.Evaluation of on-line desalter-inductively coupled plasma-mass spectro-metry system for determination of Cr(III),Cr(VI),and total chromium concentrations in natural water andurine samples[J].Spectrochimica Acta Part B:AtomicSpectroscopy,2006,61(2):230-234.
2廖自基.微量元素的环境化学及生物效应[M].北京:中国环境科学出版社,1992:288-291.
3颜世铭,洪昭毅,李增禧.实用元素医学[M].郑州:河南医科大学出版社,1999:243-249.
4 GOMEZ V,CALLAO M P.Chromium determinationand speciation since 2000[J].Trends Anal Chem,2006,25(10):1006-1015.
5 BOLZAN R C,RODRIGUES L F,de MATTOS J C P,et al.Chromium determination in pharmaceutical gradebarium sulfate by solid sampling electrothermal atomicabsorption spectrometry with Zeeman-effect backgroundcorrection[J].Talanta,2007,74(1):119-124.
6陈超,陈瑜,俞辉.微波消解石墨炉原子吸收光谱法测定胶囊和片剂用明胶中铬含量[J].分析化学,2006,34(12):1820.
7石岩,肖新月,石上梅,等.微波消解-石墨炉原子吸收法测定阿胶中铬含量[J].药物分析杂志,2011,31(8):1527.
8 European Pharmacopoeia Commission.EuropeanPharmacopoeia 7thEdition[M].European Directorate forthe Quality of Medicines,2012:707-709.
9国家药典委员会.中国药典第二部[M].北京:中国医药科技出版社,2010:1204.
10中华人民共和国卫生部.GB/T5009.123—2003食品中铬的测定[S].北京:中国标准出版社,2003.
11丁春光,朱醇,刘德晔,等.电感耦合等离子体质谱方法检测全血中30种金属及类金属元素[J].中华预防医学杂志,2012,46(8):745-749.
12王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社,2005:80-95.
13 SUN Y C,LIN C Y,WU S F,et al.Evaluation of on-line desalter-inductively coupled plasma-mass spectro-metry system for determination of Cr(III),Cr(VI),and total chromium concentrations in natural water andurine samples[J].Spectrochimica Acta Part B:AtomicSpectroscopy,2006,61(2):230-234.