Determination of Oxine-Copper Residue in Cucumis sativus L. by Dispersive Solid Phase Extraction

doi:10.3969/j.issn.1000-2561.2019.07.029

Abstract

Abstract:

A high performance liquid chromatography (HPLC) coupled with the dispersive solid phase extraction (d-SPE) method for the determination of oxine-copper residue in cucumber was established. The sample was extracted by acetonitrile and hydrochloric acid (0.1 mol/L). The extract was purified by C₁₈. The analysis was carried out by phosphate buffer saline (PBS) and sodium dodecyl sulfate (SDS) -acetonitrile (65∶35) at a flow rate of 0.6 mL/min on SunFireC₁₈(4.6×150 mm, 5 μm) column, and detected by HPLC with UV detector at a ultraviolet absorption wavelength of 250 nm. The recovery was in 92.3%-107.7% with relative standard deviation (RSD) of 2.0%-7.7% at spiked levels of 0.02, 0.2 and 2 mg/kg. The method is simple, sensitive and accurate, and could be used in the determination of oxine-copper residue in cucumber.

Key words: Cucumis sativus L., oxine-copper, dispersive solid phase extraction, high performance liquid chromatography

CLC Number:

X839.2

CHEN Siyu,WANG Mingyue,LIN Bing,LV Daizhu. Determination of Oxine-Copper Residue in Cucumis sativus L. by Dispersive Solid Phase Extraction[J]. Chinese Journal of Tropical Crops, 2019, 40(7): 1449-1454.

Figures/Tables 6

Tab. 1 Recovery and precisions of oxine-copper spiked in samples

添加浓度 Spiked level/(mg?kg^-1)	回收率 Recovery/%					平均回收率 Average recovery/%	相对标准偏差RSD/%
0.02	107.7	92.3	107.7	100.0	92.3	100.0	7.7
0.2	95.5	96.2	92.5	92.5	92.5	93.8	2.0
2	92.9	99.8	100.6	101.1	97.7	98.4	3.4

Fig. 1 Chromatogram of spiked cucumber sample (0.2 mg/kg-1)

Fig. 2 Chromatogram of blank cucumber sample with different extraction The retaintion time of oxine-copper was 6-8 min; A: Extracted by acetonitrile and hydrochloric acid (0.1 mol/L);B: Extracted by acetonitrile.

Fig. 3 Effects of concentration of hydrochloric acid on the recovery

Fig. 4 Chromatogram of oxine-copper standard (1 μg/mL) with different mobile phase A: Acetonitrile and water; B: PBS-acetonitrile; C: PBS and SDS (0.625 mmol/L)-acetonitrile; D: PBS and SDS (1.25 mmol/L)-acetonitrile.

Fig. 5 Recovery of different purification A: Multi-walled carbon nanotubes; B: Octadecylsilane and primary-secondary amine absorbent

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