基于酸性离子液体填充注射器的泡腾辅助微萃取法测定果汁样品中三嗪类除草剂

doi:10.7503/cjcu20190605

摘要/Abstract

摘要：

开发了一种高效、环保的基于酸性离子液体填充注射器的泡腾辅助微萃取法, 用于测定果汁样品中三嗪类除草剂. 萃取分散采用酸性离子液体[C₄mim][HSO₄], 它对三嗪类除草剂具有较高的溶解度, 其酸性可与碳酸盐反应产生二氧化碳, 从而加速萃取过程. 该实验的提取和分离步骤在注射器中完成, 整个预处理过程完全不需要任何设备辅助. 对碳酸氢钠用量、酸性离子液体用量、盐添加量及洗脱溶剂体积等影响萃取效率的实验条件进行了优化. 在最佳条件下, 三嗪类除草剂浓度在1~200 ng/mL范围内获得了良好的线性关系, 相关系数大于0.9984; 检出限(LOD)和定量限(LOQ)分别为0.06~0.18和0.21~0.61 ng/mL, 日间及日内精密度低于8.3%. 实验结果表明, 该方法可用于果汁样品中三嗪类除草剂的测定.

关键词: 酸性离子液体, 泡腾辅助微萃取, 三嗪除草剂

Abstract:

A rapid, efficient, eco-friendly and simple effervescence assisted microextraction method based on acidic ionic liquid packed syringe was proposed for the determination of triazine herbicides in fruit juice samples. The extraction and dispersion procedure was achieved using an acidic ionic liquid [C₄mim][HSO₄]. It possesses high solubility for triazine herbicides and acidity that can generate carbon dioxide, which accelerates the extraction procedure via reacting with carbonate. The dispersion and separation were carried out in a syringe. Thus, the whole pretreatment procedure was completely free of any equipment. A variety of experimental conditions affecting extraction efficiency, including amount of sodium bicarbonate, amount of acidic ionic liquid, salt addition and volume of elution solvent were optimized. Under the optimal conditions, good linearities were obtained in the range of 1—200 ng/mL, with coefficients better than 0.9984. The limit of detection(LOD) and limit of quantification(LOQ) varied from 0.06 to 0.18 ng/mL and 0.21 to 0.61 ng/mL, respectively. The intra-day and inter-day precisions were lower than 8.3%. The developed technique was successfully applied for determination of triazine herbicides in fruit juice samples.

Key words: Acidic ionic liquid, Effervescence assisted microextraction, Triazine herbicide

中图分类号:

O657

朴惠兰,马品一,覃祖成,姜延晓,孙颖,王兴华,宋大千. 基于酸性离子液体填充注射器的泡腾辅助微萃取法测定果汁样品中三嗪类除草剂[J]. 高等学校化学学报, 2020, 41(2): 228-234.

PIAO Huilan,MA Pinyi,QIN Zucheng,JIANG Yanxiao,SUN Ying,WANG Xinghua,SONG Daqian. Determination of Triazine Herbicides from Fruit Juice Samples Using Effervescence Assisted Microextraction Method Based on Acidic Ionic Liquid Packed Syringe[J]. Chemical Journal of Chinese Universities, 2020, 41(2): 228-234.

图/表 10

参考文献 30

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Analyte	Liner range/ (ng·mL^-1)	Regression equation	Correlation coefficient, r	LOD/ (ng·mL^-1)	LOQ/ (ng·mL^-1)	RSD(%)
Analyte	Liner range/ (ng·mL^-1)	Regression equation	Correlation coefficient, r	LOD/ (ng·mL^-1)	LOQ/ (ng·mL^-1)	Inter-day	Intra-day
Atraton	1—200	A=32273c-45035	0.9993	0.06	0.21	1.6	7.6
Desmetryn	1—200	A=22833c-32310	0.9991	0.09	0.31	6.8	7.2
Secbumeton	2—200	A=18533c-30871	0.9984	0.16	0.54	5.8	7.8
Terbumeton	2—200	A=16835c-24740	0.9990	0.18	0.61	5.4	6.9
Prometryn	1—200	A=26847c-34238	0.9990	0.06	0.18	2.9	6.3

Analyte	Liner range/ (ng·mL^-1)	Regression equation	Correlation coefficient, r	LOD/ (ng·mL^-1)	LOQ/ (ng·mL^-1)	RSD(%)
Analyte	Liner range/ (ng·mL^-1)	Regression equation	Correlation coefficient, r	LOD/ (ng·mL^-1)	LOQ/ (ng·mL^-1)	Inter-day	Intra-day
Atraton	1—200	A=32273c-45035	0.9993	0.06	0.21	1.6	7.6
Desmetryn	1—200	A=22833c-32310	0.9991	0.09	0.31	6.8	7.2
Secbumeton	2—200	A=18533c-30871	0.9984	0.16	0.54	5.8	7.8
Terbumeton	2—200	A=16835c-24740	0.9990	0.18	0.61	5.4	6.9
Prometryn	1—200	A=26847c-34238	0.9990	0.06	0.18	2.9	6.3

Matrix	Spiked/ (ng·mL^-1)	Atraton		Desmetryn		Secbumeton		Terbumeton		Prometryn
Matrix	Spiked/ (ng·mL^-1)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)
Fruit Juice	3.0	103.4	7.2	101.6	7.3	114.9	4.7	102.5	6.0	94.3	4.7
	10.0	102.4	4.6	104.0	5.8	107.7	6.5	83.0	5.3	123.2	8.2
	20.0	106.0	2.0	105.0	2.2	96.6	1.5	89.6	3.6	116.5	5.8
Tea beverage	3.0	90.4	6.9	123.5	4.4	107.6	8.7	103.2	4.0	94.4	4.6
	10.0	91.5	2.6	101.0	5.3	100.6	2.7	85.2	3.4	100.3	6.1
	20.0	96.9	5.7	119.0	6.0	112.5	6.0	93.1	5.7	100.1	6.2
Water	3.0	104.9	8.3	118.3	5.3	112.5	8.3	83.9	2.3	109.1	4.3
	10.0	96.5	2.2	102.1	7.1	99.7	7.9	80.8	7.2	104.0	5.3
	20.0	92.1	0.4	112.3	1.5	101.4	1.5	94.9	3.6	113.8	3.0

Matrix	Spiked/ (ng·mL^-1)	Atraton		Desmetryn		Secbumeton		Terbumeton		Prometryn
Matrix	Spiked/ (ng·mL^-1)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)	Recovery (%)	RSD (%)
Fruit Juice	3.0	103.4	7.2	101.6	7.3	114.9	4.7	102.5	6.0	94.3	4.7
	10.0	102.4	4.6	104.0	5.8	107.7	6.5	83.0	5.3	123.2	8.2
	20.0	106.0	2.0	105.0	2.2	96.6	1.5	89.6	3.6	116.5	5.8
Tea beverage	3.0	90.4	6.9	123.5	4.4	107.6	8.7	103.2	4.0	94.4	4.6
	10.0	91.5	2.6	101.0	5.3	100.6	2.7	85.2	3.4	100.3	6.1
	20.0	96.9	5.7	119.0	6.0	112.5	6.0	93.1	5.7	100.1	6.2
Water	3.0	104.9	8.3	118.3	5.3	112.5	8.3	83.9	2.3	109.1	4.3
	10.0	96.5	2.2	102.1	7.1	99.7	7.9	80.8	7.2	104.0	5.3
	20.0	92.1	0.4	112.3	1.5	101.4	1.5	94.9	3.6	113.8	3.0

Matrix	Analytes	Extraction method	Detection	LOD/(ng·mL^-1)	Recovery(%)	Ref.
Water	Triazine herbicides	SPME	HPLC-DAD	0.05—0.2	86.0—94.6	[25]
Water	Triazine herbicides	HF-LLLME	HPLC-DAD	0.07—0.69	85.2—113.0	[26]
Fruit juice	Triazine herbicides	CSDF-ME	HPLC-UV	0.5—1.0	71.0—90.0	[27]
Milk	Triazine herbicides	MSPE	HPLC-DAD	0.134—0.176	81.0—109.0	[28]
Milk	Triazine herbicides	SPE	HPLC-MS	0.03—0.12	82.5—97.5	[29]
Water	Pesticide residues	UA-DLLME	GC-FID	0.09—0.57	90.5—107.7	[30]
Fruit juice	Triazine herbicides	EA-DLLME	HPLC-UV	0.06—0.18	80.8—123.5	This work