Assembly of Hyphenated Instrument of Solid Phase Extraction and Solid Phase Spectroscopy and Its Application to Determination of Rhodamine B in Food
摘 要
设计并制造了以膜材料为分离富集介质的固相萃取装置和以漫反射光谱法为测定手段的测定装置相结合的自动化分析仪并应用于测定食品中罗丹明B的含量。该仪器由固相萃取装置、固相光谱测定装置和软件等3个部分组成。样品溶液(调节pH至2.00)负压自动进样,调节真空度在合适的速率下通过滤膜,待测物质富集于滤膜上。滤膜经热风干燥后由积分球在滤膜固相介质表面采集被测物质的漫反射光谱,仪器控制、光谱采集和数据处理直至报告的发出均由软件完成。在分析辣椒样品时,取样品0.500 g,用水50.0 mL超声提取10.0 min,离心后取上清液测定罗丹明B的含量。测定时用混合纤维素膜进行富集,并选择测定波长为546.7 nm。罗丹明B的线性范围为5.0~15.0 μg·L-1。分析红茶样品时,将样品用水稀释10倍后进行分析。在红茶的基质下,罗丹明B的线性范围为10.0~30.0 μg·L-1。上述2种样品的回收率为88.0%~108%,测定值的相对标准偏差(n=5)为4.6%~9.3%。
Abstract
An automatic analyzer was designed and fabricated by organic combination of solid phase extraction unit using filtering membrane as enrichment medium and diffuse reflection absorption spectrometry as detection unit, and the instrument was applied to the determination of rhodamine B in food. The analyzer consists of 3 parts:the solid phase extraction unit, the solid phase spectroscopy unit and the software. The sample solution (with its pH adjusted to 2.00) was introduced into the analyzer under reduced pressure and passed through the filtering membrane at an appropriate flow rate by adjusting the vacuum and the analytes were enriched on the membrane, which was then dried by hot air current. The information of diffuse reflection spectrometric data of the analytes was collected by the integrator from the solid phase of the dried membrane. The control conditions of the instrument, collection of spectral data, data treatment and finally the report of analytical results were completely controlled by the software. In the analysis of chilli, 0.500 g of the sample was taken and extracted ultrasonically with 50.0 mL of water for 10.0 min, and after centrifuging, the supernatant was taken for determination of rhodamine B. Mixed cellulose membrane was selected for enrichment, and the wavelength at 546.7 nm was chosen for determination. Linearity range of rhodamine B was found in the range of 5.0-15.0 μg·L-1. For analysis of red tea sample, the sample should be diluted 10 times with water. In the presence of the matrix of red tea, linearity range of rhodamine B was found in the range of 10.0-30.0 μg·L-1. Test for recovery was made by standard addition method for both the samples, giving values of recovery in the range of 88.0%-108%. Values of RSDs (n=5) found were in the range of 4.6%-9.3%.
中图分类号 O657.3 DOI 10.11973/lhjy-hx202002006
所属栏目 工作简报
基金项目 上海市科委科研计划项目(17142201100)
收稿日期 2019/3/26
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备注朱莹,硕士研究生,研究方向为光谱分析
引用该论文: ZHU Ying,LI Long,JIANG Chengde,BIAN Li,YANG Shijun,NI Chenjie,CHEN Wanchao,XIONG Qin,DU Yiping. Assembly of Hyphenated Instrument of Solid Phase Extraction and Solid Phase Spectroscopy and Its Application to Determination of Rhodamine B in Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(2): 155~160
朱莹,李龙,江成德,边丽,杨仕骏,倪晨杰,陈万超,熊芩,杜一平. 固相萃取-固相光谱联用仪的构建及其应用于食品中罗丹明B的测定[J]. 理化检验-化学分册, 2020, 56(2): 155~160
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【4】李龙,王海婷,缪文彬,等.膜富集-紫外光谱法快速检测自来水中痕量2-萘酚[J].分析测试学报, 2016,35(3):347-350.
【5】DIVRIKLI U, KARTAL A A, SOYLAK M, et al. Preconcentration of Pb(Ⅱ), Cr(Ⅲ), Cu(Ⅱ), Ni(Ⅱ) and Cd(Ⅱ) ions in environmental samples by membrane filtration prior to their flame atomic absorption spectrometric determinations[J]. Journal of Hazardous Materials, 2007,145:459-464.
【6】TAKAHASHI Y, DANWITTAYAKUL S, SUZUKI T M. Dithizone nanofiber-coated membrane for filtration-enrichment and colorimetric detection of trace Hg(Ⅱ) ion[J]. Analyst, 2009,134(7):1380-1385.
【7】杜一平,魏荷月,王蕾.固相萃取光谱(SPES)及其在光谱快检中的应用[J].光谱学与光谱分析, 2016,36(增1):333-334.
【8】LI W, WANG H T, JIANG W, et al. Multilayer and multichannel membrane filtration for separation and preconcentration of trace analytes and its application in spectral analysis[J]. Analytical Methods, 2016,8(1):129-135.
【9】杭学宇,王芹,王露,等.磁性固相萃取-石墨炉原子吸收光谱法联用分析水样中痕量镍[J].分析试验室, 2015,34(7):807-810.
【10】陈艳美,于淼.罗丹明B染色食品对人体的危害及检测[J].科学之友, 2011(18):153-153.
【11】李惠茗,李琴,赖祥文,等.石墨烯基固相萃取灵敏检测环境水样中痕量罗丹明B[J].分析试验室, 2015,34(10):1151-1154.
【12】徐声乐,王兴,刘金萍,等.罗丹明B及其在食品中检测方法研究进展[J].食品研究与开发, 2015,36(17):136-139.
【13】周鹏,余清,林钦,等.液质联用法测定辣椒红色素中罗丹明B含量[J].食品研究与开发, 2013,34(4):74-76.
【14】梁宇,黄世江,王超海,等.荧光探针法快速检测果汁中罗丹明B残留量[J].食品科学, 2012,33(18):258-260.
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