期刊
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
卷 36, 期 11, 页码 1654-1666出版社
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2019.1644458
关键词
CSHS-SAP; switchable hydrophilicity solvent; lead; GFAAS; bovine milk
资金
- National Natural Science Foundation of China [21876125, 51608341]
- Zhejiang Provincial Natural Science Foundation [LY19B070010]
- Suzhou City Science and Technology Project [SYG201815, SNG2018047, SNG2018051]
A novel microextraction method was developed by combining CO2-controlled switchable hydrophilicity solvent (SHS) with solidification of the aqueous phase (SAP), referred to as CSHS-SAP. It was applied for pre-concentration/extraction of the complexes of Pb-ammonium pyrrolidine dithiocarbamate (APDC) prior to GFAAS detection in raw bovine milk and milk products (whole-fat, half-skimmed and skimmed milks). In the CSHS-SAP microextraction, a clear interface was easily formed, and convenient and complete collection was achieved by directly transferring the SHS phase into a vial, which overcame the shortcomings of blurred interface and difficult collection of SHS phase using CSHS-based microextraction. SAP led to the increase of extraction recoveries for Pb2+ by 8-11%. Some important factors were optimised using a one-factor-at-a-time approach: 800 mu L of N,N-dimethylbutylamine and water at a ratio of 1:1 as SHS, 1.0 g L-1 APDC as chelating agent, sample pH = 6.0, 0.6 mL of 1.0 mol L-1 NaOH, solidification time of 70 min and 300 mu L of 0.5 mol L-1 HNO3 for back extraction. Under optimised conditions, limits of detection were as low as 0.01-0.02 mu g kg(-1) and enrichment factors reached more than 23-fold. Inter- and intra-day precisions had relative standard deviations of 3.6-6.4%. With the CSHS-SAP/GFAAS method Pb2+ was detected at 0.5-1.8 mu g kg(-1) in four bovine raw milk samples, which were collected from Hubei and Henan Provincial oil-producing area, China. However, Pb2+ was below the LOD in all of the local milk products. Overall, the newly developed CSHS-SAP/GFAAS method is convenient, efficient and robust, giving it great potential for rapid and accurate analysis of trace Pb2+ in liquid milks.
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