Analysis of four preservatives in beverages and instant noodle samples by high performance liquid chromatography-ultraviolet detection coupled with magnetic solid phase extraction based on metal-organic frameworks

doi:10.3724/SP.J.1123.2019.06014

Abstract

Abstract:

Magnetic amino functionalized metal-organic frameworks (MOFs) were prepared by a simple stirring and blending process. The obtained composites had good magnetic and thermal stability with a large specific surface area, and were used for the extraction of four preservatives with different polarities (benzoic acid, sorbic acid, propyl p-hydroxybenzoate and butyl p-hydroxybenzoate) in soda water, vitamin beverage and instant noodle cake samples. After optimizing the conditions for magnetic solid phase extraction (MSPE) and desorption, the four preservatives were analysed by a high performance liquid chromatography-ultraviolet detection (HPLC-UV) method. The analytes were separated on a Purospher^® STAR LP C18 column (250 mm×4.6 mm, 5 μm). Methanol and 10 mmol/L ammonium acetate aqueous solution (50:50, v/v) were used as the mobile phases with gradient elution. The limits of detection of the four preservatives were 0.51-1.89 μg/L. The recoveries of the target preservatives were 72.2%-109% in the soda water, vitamin beverage and instant noodle cake samples. The method is simple, rapid, accurate and reliable, and is suitable for the analysis of preservatives with different polarities in beverages and foods. The method can provide an effective technology for food safety and quality control.

Key words: high performance liquid chromatography (HPLC), magnetic solid phase extraction (MSPE), metal-organic frameworks (MOFs), preservatives, beverages, instant noodles

XIAO Zuowei, HE Man, CHEN Beibei, HU Bin. Analysis of four preservatives in beverages and instant noodle samples by high performance liquid chromatography-ultraviolet detection coupled with magnetic solid phase extraction based on metal-organic frameworks[J]. Chinese Journal of Chromatography, 2020, 38(1): 127-136.

Figures/Tables 10

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Analyte	Linear range/(μg/L)	r	LOD/(μg/L)	LOQ/(μg/L)	RSDs (n=7)/%		EF
Analyte	Linear range/(μg/L)	r	LOD/(μg/L)	LOQ/(μg/L)	Intra-day	Inter-day	EF
BA	2-2000	0.9998	0.51	1.60	3.8	3.3	40.2
SA	2-1000	0.9976	0.65	2.28	5.5	7.4	19.1
PP	10-1000	0.9982	1.89	5.35	3.5	7.8	6.3
BP	5-1000	0.9961	1.29	4.02	2.1	6.7	15.9

Analyte	Linear range/(μg/L)	r	LOD/(μg/L)	LOQ/(μg/L)	RSDs (n=7)/%		EF
Analyte	Linear range/(μg/L)	r	LOD/(μg/L)	LOQ/(μg/L)	Intra-day	Inter-day	EF
BA	2-2000	0.9998	0.51	1.60	3.8	3.3	40.2
SA	2-1000	0.9976	0.65	2.28	5.5	7.4	19.1
PP	10-1000	0.9982	1.89	5.35	3.5	7.8	6.3
BP	5-1000	0.9961	1.29	4.02	2.1	6.7	15.9

Method	Analytes	Samples	Extraction time/min	LOD/ (μg/L)	Recovery/ %	Ref.
DLLME: dispersive liquid liquid microextraction; CLC: capillary liquid chromatography; HKUST-1: a kind of MOFs materials; d- μ SPE: dispersive micro-solid-phase extraction; CME: capillary microextraction; SCSE: stir cake sorptive extraction; PDMS: polydimethylsiloxane; SBSE: stir bar sorptive extraction; MSPE: magnetic solid phase extraction.
DLLME-CLC-MS	MP, EP, PP, BP	human urine, serum	20	7-11	95.2-107	[34]
HKUST-1-d-μSPE-HPLC-UV	MP, EP, PP, BP	cosmetic creams, human urine	5	0.1-0.6	63.7-121	[22]
Monolith-CME-HPLC-UV	BA, SA	soft drinks	5	0.9-1.2	84.4-106	[18]
Monolith-SCSE-HPLC-UV	BA, SA	juices, soft drinks	180	0.16-1.03	96.1-104	[6]
PDMS-SPE-GC-FID	BA, SA, MP, EP, PP	soft drinks, yogurts, sauces	45	2-200	92-106	[12]
Dual phase-dual SBSE-HPLC-UV	BA, SA, MP, EP, PP, BP	cola, orange juice, herb tea	40	0.6-2.7	74.6-119	[21]
UiO-66-NH₂-MSPE-HPLC-UV	BA, SA, PP, BP	beverages, instant noodles	10	0.51-1.89	59.2-109	this work

Method	Analytes	Samples	Extraction time/min	LOD/ (μg/L)	Recovery/ %	Ref.
DLLME: dispersive liquid liquid microextraction; CLC: capillary liquid chromatography; HKUST-1: a kind of MOFs materials; d- μ SPE: dispersive micro-solid-phase extraction; CME: capillary microextraction; SCSE: stir cake sorptive extraction; PDMS: polydimethylsiloxane; SBSE: stir bar sorptive extraction; MSPE: magnetic solid phase extraction.
DLLME-CLC-MS	MP, EP, PP, BP	human urine, serum	20	7-11	95.2-107	[34]
HKUST-1-d-μSPE-HPLC-UV	MP, EP, PP, BP	cosmetic creams, human urine	5	0.1-0.6	63.7-121	[22]
Monolith-CME-HPLC-UV	BA, SA	soft drinks	5	0.9-1.2	84.4-106	[18]
Monolith-SCSE-HPLC-UV	BA, SA	juices, soft drinks	180	0.16-1.03	96.1-104	[6]
PDMS-SPE-GC-FID	BA, SA, MP, EP, PP	soft drinks, yogurts, sauces	45	2-200	92-106	[12]
Dual phase-dual SBSE-HPLC-UV	BA, SA, MP, EP, PP, BP	cola, orange juice, herb tea	40	0.6-2.7	74.6-119	[21]
UiO-66-NH₂-MSPE-HPLC-UV	BA, SA, PP, BP	beverages, instant noodles	10	0.51-1.89	59.2-109	this work

Compound	Added/ (μg/L)	Soda water		Vitamin beverage		Instant noodles
Compound	Added/ (μg/L)	Found/ (μg/L)	Recovery/ %	Found/ (μg/L)	Recovery/ %	Found/ (μg/L)	Recovery/ %
ND: not detected; -: no data.
BA	0	ND	-	ND	-	ND	-
	5.00	4.11±0.3	82.3	3.67±0.2	73.4	4.68±0.2	93.6
	25.0	24.9±1.2	99.6	20.3±1.4	81.2	24.2±1.0	96.6
	50.0	47.9±1.7	95.7	44.7±2.2	89.4	51.3±2.1	103
SA	0	ND	-	ND	-	ND	-
	5.00	4.57±0.2	91.5	3.61±0.4	72.2	4.3±0.2	85.9
	25.0	27.3±0.9	109	20.0±1.3	80.1	23.6±1.5	94.3
	50.0	53.5±1.9	107	42.9±1.7	85.8	46.9±1.6	93.9
PP	0	ND	-	ND	-	ND	-
	10.0	7.46±0.8	74.6	7.55±0.5	75.5	8.01±0.2	80.1
	50.0	39.7±1.5	79.3	37.5±1.2	74.9	43.2±2.2	86.4
	100	84.6±3.9	84.6	80.2±2.3	80.2	83.5±4.1	83.5
BP	0	ND	-	ND	-	ND	-
	10.0	8.79±0.4	87.9	8.25±0.6	82.5	9.78±0.4	97.8
	50.0	48.2±1.0	96.5	43.7±1.5	87.3	47.2±1.6	94.3
	100	89.1±4.2	89.1	94.2±6.4	94.2	89.2±5.3	89.2