塞曼火焰原子吸收与石墨炉原子吸收法测定明胶空心胶囊壳中铬的方法比较

目的: 研究塞曼效应背景校正的火焰和石墨炉原子吸收法测定胶囊中铬的影响。 方法: 采用微波消解仪对胶囊壳样品进行消解,在波长359.3 nm下,灯电流7.5 mA;狭缝宽1.3 nm,塞曼背景校正,分别采用塞曼火焰原子吸收和石墨炉原子吸收法进行测定。 结果: 火焰原子吸收法:线性范围0.04~1.0 mg·mL^-1;相关系数为0.9998,检测限5.26 ng·mL^-1,RSD为0.68%~1.0%,加样回收率为100.0%~116.7%;石墨炉原子吸收法:线性范围为1~20 ng·mL^-1,相关系数为0.9998,检测限为0.26 ng·mL^-1,RSD为1.7%~4.9%,加样回收率为98.2%~105.6%。 结论: 塞曼火焰原子吸收法简便、快捷,能满足大量样品筛选及企业内部质控筛选与定值;石墨炉原子吸收法检测限较前者低,准确度较高。

Objective: To investigate effects of Zeeman flame atomic absorption spectrophotometry (AAS) and graphite furnace AAS on the determination of chromium in capsule shells. Methods: Microwave digestion was adopted to digest the capsule shells.Zeeman effect was used in the background correction.The slit width was set at 1.3 nm,lamp current 7.5 mA,and the content of chromium was determined at a wavelength of 359.3 nm by Zeeman flame AAS and graphite furnace AAS respectively. Results: For the Zeeman flame AAS method,the calibration curve was linear in the range of 0-1.0 μg·mL^-1 (r=0.9998),the detection limit was 5.26 ng·mL^-1,RSD was 0.68%-1.0% and the average recovery was 100.0%-116.7%.For the graphite furnace AAS method,the calibration curve was linear in the range of 0-20 ng·mL^-1 (r=0.9999),the detection limit was 0.26 ng·mL^-1,RSD was 1.7%-4.9% and the average recovery was 98.2%-105.6%. Conclusion: The Zeeman flame AAS method is simple,fast,and suitable for the preliminary determination of chromium in capsule shells in emergent cases;the graphite furnace AAS method is sensitive,accurate,and suitable for the determination of chromium in capsule shells in any case.

1 GhP(中国药典).2010.Vol Ⅱ(二部):1204
2 GB(中华人民共和国国家标准).6783-94,Food Additive Gelatine(食品添加剂明胶)
3 QB(中华人民共和国轻工行业标准).2354-2005,Pharmaceutical Gelatine(药用明胶)
4 Ebdon L,Pitts L,Cornelis R,et al.Trace Element Speciation for Environment,Food and Health.UK. Cambrige:Royal Soeiety of Chemistry,2001.244
5 LIU G.Applications and safety issues of gel in the use of pharmaceutical and food industry.Gel Sci Technol,2002,22(4):169
6 Mandiwana KL,Panichev N,Panicheva S.Determination of chromium(VI) in black,green and herbal teas.Food Chem,2011,129(4):1839
7 YU Hui(俞辉),CHEN Chao(陈超),CHEN Yu(陈瑜).Determination of Cr in vacant capsules by graphite furnace atomic absorbance spectrometry (石墨炉原子吸收分光光度法检测空心胶囊中铬元素的含量).Chin J Pharm Anal(药物分析杂志),2006,26 (11):1644
8 DONG Zhe(董喆),FENG Ke-ran(冯克然),ZHANG Lu-yong(张露勇).Determination of chromium in soft gel by microwave digestion-graphite furnace atomic absorption spectrophotometry (微波消解-石墨炉原子吸收法测定软胶囊壳中重金属铬的方法学研究).Chin Pharm J(中国药学杂志),2012,47(9):717
9 GB/T(中华人民共和国国家标准).5009.123-2003,Determination of chromium in foods(食品中铬的测定)
10 JIA Ai-ling (贾艾玲),WANG Hong-mei(王红梅),LI Ling-ling(李玲玲).ICP-MS determination of 6 hazard elements in Colla Corii Asini(Ejiao) (电感耦合等离子体质谱法检测阿胶中6种有害元素的含量).Chin J Pharm Anal(药物分析杂志),2012,32 (3):434
11 YAN Qing-hua(闫清华),YANG Li(杨理),YANG Li-juan(杨利娟).Determination of constant and trace elements in six herbal drugs for relieving heat and toxic by microwave digestion with ICP-AES(微波消解ICP-AES检测6种清热解毒类中草药中14种常微量元素).Chin J Pharm Anal(药物分析杂志),2011,31 (7):1393
12 ChP(中国药典).2010.Vol Ⅱ(二部):Appendix(附录)Ⅳ D