纳米固相微萃取应用于干红辣椒、水果饮料及红酒中罗丹明B的定量分析

doi:10.7503/cjcu20160873

高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (6): 935.doi: 10.7503/cjcu20160873

• 中国第四届静电纺丝大会专题研究论文 • 上一篇下一篇

纳米固相微萃取应用于干红辣椒、水果饮料及红酒中罗丹明B的定量分析

卫兰兰¹, 晏嫣², 康学军³()

1. 东南大学环境医学与工程教育部重点实验室, 南京 210096
2. 江苏产品质量检验研究院, 南京 210000
3. 东南大学儿童发展与学习科学教育部重点实验室, 南京 210096

收稿日期:2016-12-05 出版日期:2017-06-10 发布日期:2017-05-23
作者简介:联系人简介: 康学军, 女, 博士, 教授, 主要从事生物分析化学方面的研究. E-mail: xjkang64@163.com
基金资助:
国家自然科学基金(批准号: 81172720, 81673230)、苏州科技局基金(批准号: ZXG201441)、江苏省社会发展研究项目(批准号: BE2016741)和中央高校基本科研专项资金(批准号: KYLX15_0220)资助.

Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Dry Chilli, Fruit Drink and Red Wine

WEI Lanlan¹, YAN Yan², KANG Xuejue^3,^*()

1. Key Laboratory of Environmental Medicine and Engineering(Ministry of Education), School of Public Health,Southeast University, Nanjing 210096, China
2. Jiangsu Product Quality Testing & Inspection Institute, Nanjing 210000, China;
3. Key Laboratory of Child Development and Learning Science of Ministry of Education,Research Center for Learning Science, Southeast University, Nanjing 210096, China

Received:2016-12-05 Online:2017-06-10 Published:2017-05-23
Contact: KANG Xuejue E-mail:xjkang64@163.com
Supported by:
This paper is supported by the National Natural Science Foundation of China(Nos.81172720, 81673230), the Suzhou Science and Technology Department Foundation, China(No.ZXG201441), the Social Development Research Program of Jiangsu Provincial Science and Technology Department, China(No.BE2016741) and the Fundamental Research Funds for the Central Universities, Colleges and Universities in Jiangsu Province Plans to Graduate Research and Innovation Projects, China(No.KYLX15_0220).

摘要/Abstract

摘要：

制备了一种新型的聚苯乙烯纳米纤维, 将其作为固相萃取吸附剂装填制成固相萃取柱, 与高效液相色谱联用建立了干辣椒、水果饮料及红酒中罗丹明B的定量分析方法. 高效液相色谱以3 g/L磷酸缓冲液-甲醇混合溶液(体积比3∶7, pH=7.0)为流动相. 通过对提取条件的优化, 得到该方法对干辣椒中罗丹明B的检出限为0.1 ng/g, 最低定量限为0.6 ng/g; 对水果饮料和红酒中罗丹明B的检出限均为0.2 ng/mL, 最低定量限均为0.5 ng/mL. 此方法对干辣椒中罗丹明B的提取回收率为98.2%~110.3%; 对水果饮料中罗丹明B的提取回收率为94.6%~102.2%; 对红酒中罗丹明B的提取回收率为90.4%~104.6%. 该方法的线性范围为1~100 ng/mL(ng/g), 相对标准偏差为2.3%~9.0%. 该方法灵敏度高、选择性好, 可用于干辣椒、水果饮料及红酒中罗丹明B的定量分析.

关键词: 罗丹明B, 纳米纤维, 固相微萃取

Abstract:

A method for the determination of Rhodamine B in dry chilli, fruit drink and red wine was developed and validated. The analyte was extracted with acetonitrile from foodstuffs. A novel electrospun polymer nanofibers packed micro-column was used for cleaning and concentrating the Rhodamine B in these foodstuffs. High performance liquid chromatography with fluorescence detection(HPLC-Flu) was used for the determination of Rhodamine B in the samples. The mobile phase was composed of 3 g/L phosphate buffer and methanol(3∶7, volume ratio), the pH was adjusted to 7.0 with orthophosphoric acid. The results showed that the standard curve was linear over the validated concentrations range of 1—100 ng/mL(ng/g), and the limit of detection(LOD) for Rhodamine B spiked samples was 0.1 ng/g in dry chilli, 0.2 ng/mL in both fruit drink and red wine. The limit of quantitation(LOQ) for Rhodamine B spiked into dry chilli was 0.6 ng/g, fruit drink 0.5 ng/mL and red wine 0.5 ng/mL, respectively. The average recoveries of Rhodamine B were 98.2%—110.3% for dry chilli, 94.6%—102.2% for fruit drink, and 90.4%—104.6% for red wine, respectively. The relative standard deviation of the method was 2.3%—9.0%. This proposed method was applied to real samples including dry chilli, fruit drink as well as red wine, and there was no Rhodamine B found in fruit drink or red wine, but Rhodamine B was found in chilli powder.

Key words: Rhodamine B, Nanofibers, Solid-phase extraction

中图分类号:

O655

TrendMD:

卫兰兰, 晏嫣, 康学军. 纳米固相微萃取应用于干红辣椒、水果饮料及红酒中罗丹明B的定量分析. 高等学校化学学报, 2017, 38(6): 935.

WEI Lanlan, YAN Yan, KANG Xuejue. Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Dry Chilli, Fruit Drink and Red Wine. Chem. J. Chinese Universities, 2017, 38(6): 935.

图/表 10

Fig.1 Array SPE extraction device(A) and PFSPE column(B)

Fig.2 Effects of extracting solvents on the extraction efficiency

Fig.3 Effects of pH values on the extraction efficiency

Fig.4 Effects of various eluents on the recoveries of Rhodamine B a. 100 μL acetonitrile; b. 100 μL ethanol; c. 50 μL methanol;d. 100 μL methanol; e. 200 μL methanol.

Table 1 Linearity for Rhodamine B in the samples

Sample	Linear equation	Correlation, R²	Linear range/(ng·g^-1 or ng·mL^-1)
Dry chilli	y=7290.6x+11443	0.9941	1—100
Fruit drink	y=4587.9x+9277.7	0.9993	1—100
Red wine	y=4965.8x+629.8	0.9998	1—100

Table 2 Methodological parameters for determination of Rhodamine B(n=3)

Sample	Spiking level/ (ng·g^-1 or ng·mL^-1)	Recovery(%)			RSD(%)	LOD/(ng·g^-1 or ng·mL^-1)	LOQ/(ng·g^-1 or ng·mL^-1)
Dry chilli	5	97.3	98.2	108	7.9	0.1	0.6
	50	114.13	113.9	102.7	4.1
	100	99.6	97.3	97.7	3.9
Fruit drink	5	94.9	109.9	89.8	9.3	0.2	0.5
	50	110.1	83.1	90.7	4.7
	100	103.8	99.8	103.1	2.1
Red wine	5	110.1	101.2	102.5	9.0	0.2	0.5
	50	94.5	93.1	83.7	7.2
	100	105	104.3	100.8	2.3

Table 3 Comparison with commercial SPE columns

Column	ODS-SPE(vimins)	Sep-pak C₁₈ column(waters)	Packed-nanofiber
Organic solvent/mL	15	15	0.5
Time spent/h	3	3	0.5
Extraction recovery(%)	69.8	79.8	85.0

Fig.5 HPLC-Flu chromatograms of the real samples a. Chilli powder; b. standard solution of Rhodamine B; c. red wine; d. dry chill; e. fruit drink.

Fig.6 PDA spectra of Rhodamine B in real sample(A) and Rhodamine B standard solution(B)

Fig.7 LC-MS/MS chromatograms of Rhodamine B in different matrix (A) Blank; (B) real sample; (C) standard solution.

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纳米固相微萃取应用于干红辣椒、水果饮料及红酒中罗丹明B的定量分析

Application of Packed-nanofibers Solid-phase Extraction for Determination of Rhodamine B in Dry Chilli, Fruit Drink and Red Wine

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