在注射器内棉纤维支撑的液相萃取结合气相色谱-串联质谱法测定食用油中的游离 3-单氯-1,2-丙二醇。
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.
机构信息
Key Laboratory of Targeting Therapy and Diagnosis for Critical Diseases of Henan Province, School of Pharmaceutical Sciences, Zhengzhou University, Zhengzhou, Henan, China.
Department of Pharmacy, the First Affiliated Hospital of Zhengzhou University, Zhengzhou, Henan, China; Henan Engineering Research Center of Clinical Mass Spectrometry for Precision Medicine, Zhengzhou, Henan, China.
出版信息
J Chromatogr A. 2022 Jun 21;1673:463081. doi: 10.1016/j.chroma.2022.463081. Epub 2022 Apr 21.
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 (R) 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.
在本研究中，天然棉纤维被用作水的载体，而水则作为低极性食用油中极性成分的液相微萃取提取剂。构建了一种注射器内萃取装置，通过在注射器针头和塑料注射器管之间装入一定量的棉纤维，便于萃取过程，然后通过推拉注射器柱塞方便地进行萃取过程。它可以被视为一种新型的动态液相微萃取方法，同时操作更加方便。为了进行可行性研究，将新型注射器内棉纤维支撑液萃取（CF-SLE）预处理方法应用于食用油中游离 3-单氯-1,2-丙二醇（3-MCPD）的提取。具体来说，通过成功地推拉 1 mL 水和 1 mL HEX 各两次，使棉纤维支撑一定量的水。然后，将 2.0 mL 稀释的油样（含 0.4 g 油）装入并抽出四次进行萃取，在此过程中，3-MCPD 被萃取到支撑水中。用 1 mL 乙酸乙酯（EA）将提取的 3-MCPD 解吸，用三甲基硅烷咪唑（TMSI）衍生化，并用气相色谱-串联质谱（GC-MS/MS）分析。对于三种不同的添加食用油，内标归一化基质效应（IS-normalized ME）值在 96.3-104.8%范围内，相对标准偏差（RSD）为 4.3%，有利于准确的定量分析。定量限（LOQ）计算为 2 ng/g，满足食用油中 3-MCPD 的常规测定要求。在 2-500 ng/g 范围内得到了满意的线性，相关系数（R）为 0.998。相对回收率在 96.9-110.5%范围内。日内和日间 RSD 分别小于 8.2%和 10.2%。该方法为测定食用油中游离 3-MCPD 提供了一种高效、简单、低成本且易于自动化的策略。
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