School of Food Science and Engineering, Shandong Academy of Sciences, Qilu University of Technology, Jinan, P. R. China.
Institute of Food & Nutrition Science and Technology, Shandong Academy of Agricultural Sciences, Jinan, P. R. China.
J Sep Sci. 2023 Jun;46(11):e2200910. doi: 10.1002/jssc.202200910. Epub 2023 Apr 12.
3-Chloro-1,2-propanediol is a common food contaminant, but reports on its determination in biological tissues are lacking. In the present study, a method was developed to detect 3-chloro-1,2-propanediol contents in rat tissues by quick-easy-cheap-effective-rugged-and-safe extraction and gas chromatography-mass spectrometry analysis. Biological samples were extracted with ethyl acetate and purified with adsorbents. The optimized adsorbent for each sample was selected from 4-5 combinations of N-propylethylenediamine, octadecylsilane, graphitized carbon black, strong anion exchange, and florisil. Extracted 3-chloro-1,2-propanediol was derivatized with heptafluorobutyric anhydride and subjected to gas chromatography-mass spectrometry. This method had good linearity (correlation coefficients >0.99) in the range of 2-2000 ng/g for blood, kidney, liver, testis, and brain samples. The limits of detection were under 0.8 ng/g; the limits of quantification were 2 ng/g; the recovery rates were 85%-102%; and the matrix effects were 1.98%-7.67%. This method also had good precision. The dynamic changes in 3-chloro-1,2-propanediol in rats gavaged with 20 mg/kg b.w. for 24 h were detected using this method. The 3-chloro-1,2-propanediol content in each tissue sharply increased to a peak, rapidly decreased within 2 h, and stabilized at 12 h. 3-Chloro-1,2-propanediol persisted in the kidney, testis, and liver 24 h after gavage.
3-氯-1,2-丙二醇是一种常见的食品污染物,但有关其在生物组织中测定的报道很少。本研究建立了一种快速、简便、经济、有效、耐用和安全的提取方法,并结合气相色谱-质谱分析检测大鼠组织中 3-氯-1,2-丙二醇含量的方法。生物样品用乙酸乙酯提取,用吸附剂净化。从 N-丙基乙二胺、十八烷基硅烷、石墨化炭黑、强阴离子交换和弗罗里硅土 4-5 种组合中选择每种样品的最佳吸附剂。提取的 3-氯-1,2-丙二醇用七氟丁酰酐衍生化,然后进行气相色谱-质谱分析。该方法在血液、肾脏、肝脏、睾丸和脑组织样品中 2-2000ng/g 的范围内具有良好的线性(相关系数>0.99)。检测限低于 0.8ng/g;定量限为 2ng/g;回收率为 85%-102%;基质效应为 1.98%-7.67%。该方法还具有良好的精密度。用该方法检测了大鼠灌胃 20mg/kg bw 24 h 后 3-氯-1,2-丙二醇的动态变化。各组织中 3-氯-1,2-丙二醇含量迅速增加至峰值,2 h 内迅速下降,12 h 时稳定。灌胃 24 h 后,3-氯-1,2-丙二醇仍存在于肾脏、睾丸和肝脏中。