In-syringe cotton fiber-supported liquid extraction coupled with gas chromatography-tandem mass spectrometry for the determination of free 3-mono-chloropropane-1,2-diol in edible oils

【作者】Chen, Di; Zhang, Man-Yu; Bu, Xin-Miao; Wang, Bin; Xu, Xin-Li; Yang, Sen; Sun, Zhi*; Xu, Xia*

【期刊名】Journalof Chromatography A

【影响因子】2021年: 4.601

【作者单位】Key Laboratory of Targeting Therapy and Diagnosis for Critical Diseases of Henan Province, School of Pharmaceutical Sciences, Zhengzhou University, 100 Kexue Avenue, Zhengzhou 450001, PR China

【年，卷(期)：页码】2022, 1667: 462891

【关键词】In-syringe; Cotton fiber-supported liquid extraction;  3-Mono-chloropropane-1,2-diol; Edible oil; GC-MS/MS

【摘要】In the current study, natural cotton fiber was served as the supporter of water, and the water acted as an extractant for liquid-phase microextraction of polar components in low-polar edible oils. An in-syringe extraction device was constructed to facilitate the extraction process by simply loading a certain amount of cotton fibers between the syringe needle and the plastic syringe tube. Then, the extraction process can be conveniently conducted by pull-push the syringe plunger. It can be regarded as a new type of dynamic liquid-phase microextraction method while operated more convent. For the feasibility study, the novel in-syringe cotton fiber-supported liquid extraction (CF-SLECF-SLE) pretreatment method was applied to extract free 3-mono-chloropropane-1,2-diol (3-MCPD) in edible oils. Specifically, the cotton fibers supported a certain amount of water by successfully pulling-pushing 1 mL of water and 1 mL of HEX in/out twice, respectively. Then, 2.0 mL of diluted oil sample (containing 0.4 g oil) was loaded in and out four times for extraction, during which process 3-MCPD was extracted into the supported water. The extracted 3-MCPD was desorbed with 1 mL of ethyl acetate (EA), derivatized with trimethyl silane imidazole (TMSI), and analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS). For three different spiked edible oils, the internal standard normalized matrix effect (IS-normalized ME) values were in ranges of 96.3–104.8% with RSD being 4.3%, benefiting the accurate quantitative analysis. The limit of quantification (LOQ) was calculated to be 2 ng/g, which met the regular determination requirement of 3-MCPD in edible oils. Satisfied linearity was obtained in 2–500 ng/g, with correlation coefficients (R2) being 0.998. The relative recoveries were in the ranges of 96.9–110.5%. The intra-/inter-day RSDs were less than 8.2% and 10.2%, respectively. The proposed method provides an efficient, simple, low-cost, and easy to automate strategy for determining free 3-MCPD in edible oils.

【全文链接】https://www.sciencedirect.com/science/article/pii/S0021967322002746