表面增强拉曼光谱快速检测蜂蜜中的金霉素残留

doi:10.7503/cjcu20180016

摘要/Abstract

摘要：

利用表面增强拉曼光谱(SERS)技术对蜂蜜中的金霉素(CTC)残留进行了快速、无损检测. 以自制的金纳米粒子作金霉素的拉曼增强基底, 对金纳米粒子与金霉素混合体积比及混合时间进行了讨论与优化, 检测了不同浓度梯度的金霉素标准溶液, 绘制了特征峰处浓度-拉曼信号强度的线性方程, 对蜂蜜进行前处理后, 运用加标回收法考察其回收率. 结果表明, 金霉素溶液在1450 cm^-1处的特征峰可以作为蜂蜜中金霉素残留量检测的特征峰, 金纳米基底和金霉素标准液的最佳混合体积比为1:1, 最佳混合时间为1 min. 金霉素的浓度(X)在10~250 mg/L范围内与其在1450 cm^-1处的SERS特征峰强度(Y)有着良好的线性关系, 线性方程为Y=1×10^-4X+0.0110(R²=0.9948). 检测实际蜂蜜样品中金霉素含量的加标回收率均在80%~120%之间. 该检测方法操作简单、快捷、准确度高, 为检测食品中抗生素残留提供了新的思路和方法.

关键词: 表面增强拉曼光谱, 金纳米粒子, 金霉素, 蜂蜜

Abstract:

The surface-enhanced Raman spectroscopy(SERS) technique was used to rapidly and non-destructively detect the residues of chlortetracycline(CTC) in honey. The prepared gold nanoparticles were used as Raman signal enhancement module. The influence of volume ratio and interact time between gold nanoparticles and CTC was discussed and optimized. Different concentrations of CTC solution were detected. The linear equation of concentration and Raman signal strength on characteristic peak was drawing. After pretreated, the recovery rate of honey sample was detected by the recovery of standard addition. The results show that the characteristic peak of chlortetracycline in 1450 cm^-1 could be used to detecting chlortetracycline(CTC) residues in honey. The best volume ratio of gold nanoparticle to CTC was 1:1 and the best interact time was 1 min. Within the scope of 10—250 mg/L, there was a favorable linearity between the concentration of CTC and SERS characteristic peak in 1450 cm^-1. Linear equation was Y=1×10^-4X+0.0110, and the coefficient of determination was 0.9948. Recovery rate was from 80% to 120% when detecting chlortetracycline(CTC) residues in honey. This detection method is simple, fast, and accurate which provides a new method for detecting antibiotic residues in foods.

Key words: Surface-enhanced Raman scattering(SERS), Au nanoparticle, Chlortetracycline(CTC), Honey

中图分类号:

O657.3

TrendMD:

张璐涛, 周光明, 罗丹, 陈蓉. 表面增强拉曼光谱快速检测蜂蜜中的金霉素残留. 高等学校化学学报, 2018, 39(8): 1662.

ZHANG Lutao, ZHOU Guangming, LUO Dan, CHEN Rong. Rapid Detection on Chlortetracycline Residues in Honey by Surface-enhanced Raman Spectroscopy^†. Chem. J. Chinese Universities, 2018, 39(8): 1662.

图/表 9

Fig.1 UV-Vis absorption spectra of Au NPs(a) and Au NPs-CTC(b)

Fig.2 SEM images of Au NPs(A) and Au NPs-CTC solution(B)

Fig.3 Raman spectra of the solid CTC(a) and the SERS(b) and RRS(c) of the CTC solution

Fig.4 SERS of CTC with different volume ratio of CTC to Au NPsa. 1:1; b. 2:1; c. 1:2; d. 1:3; e. 3:1.

Fig.5 SERS of CTC with different mix duration between CTC and Au NPs(A) and variation of SERS standard peak intensity along with increasing mixing time of CTC and Au NPs(B)

Fig.6 SERS of CTC solution with different concentrationsc(CTC)/(mg·L-1): a. 10; b. 50; c. 100;d. 150; e. 200; f. 250.

Table 1 Comparison of parameters and linear quations at diffferent Raman shift

Raman shift/ cm^-1	Linear equation	R²	SE
745	Y=1×10^-4X+0.0070	0.9868	1.189×10^-3
849	Y=1×10^-4X+0.0063	0.9824	1.337×10^-3
935	Y=1×10^-4X+0.0073	0.9878	1.354×10^-3
1002	Y=9×10^-5X+0.0067	0.9890	1.125×10^-3
1450	Y=1×10^-4X+0.0110	0.9948	1.035×10^-3

Fig.7 Liner regression curve about change of SERS signal of CTC in characteristic peak along with concentration of CTC

Table 2 Recovery experiment of two different kinds of honey

Sample	No.	Added concentration of CTC/ (mg·L^-1)	Detection of CTC concentration/ (mg·L^-1)	Recovery rate(%)
Honey(homemade)	1	0	0	—
	2	0.50	0.476—0.519	95—103
	3	1	0.896—0.997	89—99
Honey(purchased)	1	0	0	—
	2	0.50	0.459—0.495	91—99
	3	1	0.957—1.055	95—105

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