•  
  •  
 

Corresponding Author(s)

冯燕英（1993—），女，湖南省产商品质量检验研究院助理工程师，硕士。E-mail:307351506@qq.com

Abstract

Objective: To establish a new accurate method for the determination of mineral oil saturated hydrocarbon （MOSH） in infant formula by solid phase extraction combined with gas chromatography-Flame Ionization Detection （SPE-GC-FID）. Methods: Different extraction methods such as soaking extraction, oscillating extraction, ultrasonic assisted extraction, liquid-liquid extraction were used to extract MOSH from infant formula milk powder, and different extraction solvents such as n-hexane, isooctane, benzene, mixed solvents were used to extract MOSH. The optimal extraction method and extraction solvent were determined based on the extraction amount of MOSH. The target compounds purified by AgNO3 SPE column, and finally detected by gas chromatography-Flame Ionization Detection （GC-FID）. Results: The calibration curve of MOSH was linear in the range of 10.0～1 000 μg/mL with correlation coefficient of 0.999 97. The limit of detection was 1.0 mg/kg, and the limit of quantitation was 3.0 mg/kg. The recoveries from spiked samples were 93.3%～103.7%, and the relative standard deviations were 2.3%～5.9%. The MOSH in 8 commercially available infant formula was detected by the established method, and the results were between 1.06 and 9.83 mg/kg, indicating that there was a certain risk of MOSH contamination in infant formula. Conclusion: This method is accurate, sensitive, and suitable for the detection of MOSH in infant formula.

Publication Date

12-26-2023

First Page

69

Last Page

74

DOI

10.13652/j.spjx.1003.5788.2023.60108

References

[1] World Health Organization. Evaluation of certain food additives[J]. World Health Organization Technical Report Series, 2012（974）: 1-183.
[2] BIEDERMANN M, GROB K. How "white" was the mineral oil in the contaminated Ukrainian sunflower oils[J]. European Journal of Lipid Science and Technology, 2009, 111（4）: 313-319.
[3] GROB K. Update on recycled paperboard and its compliance for food contact[J]. Journal of Consumer Protection and Food Safety, 2014, 9（3）: 213-219.
[4] European Food Safety Authority （EFSA）. Scientific opinion on mineral oil hydrocarbons in food[J]. EFSA Journal, 2012, 10（6）: 2 704.
[5] NYGAARD U C, VEGE A, ROGNUM T, et al. Toxic effects of mineral oil saturated hydrocarbons （MOSH） and relation to accumulation in rat liver[J]. Food and Chemical Toxicology: An International Journal Published for the British Industrial Biological Research Association, 2023, 177: 113847.
[6] LIU L L, LI B N, YANG D Y, et al. Survey of mineral oil hydrocarbons in Chinese commercial complementary foods for infants and young children[J]. Food Additives & Contaminants: Part A, 2021, 38（9）: 1 441-1 455.
[7] ANA S, LARA G, CHIARA C, et al. Mineral oil contamination in basil pesto from the Italian market: Ingredient contribution and market survey[J]. Journal of Food Composition and Analysis, 2023, 115: 104914.
[8] NESTOLA M. Automated workflow utilizing saponification and improved epoxidation for the sensitive determination of mineral oil saturated and aromatic hydrocarbons in edible oils and fats[J]. Journal of Chromatography A, 2022, 1 682: 463523.
[9] SUI H X, GAO H B, CHEN Y F, et al. Survey of mineral oil hydrocarbons in infant formula from the Chinese market[J]. Food Additives & Contaminants: Part A, 2020, 37（6）: 1 040-1 048.
[10] HOCHEGGER A, MORET S, GEURTS L, et al. Mineral oil risk assessment: Knowledge gaps and roadmap. Outcome of a multi-stakeholders workshop[J]. Trends in Food Science & Technology, 2021, 113: 151-166.
[11] NICOLA S, MAURINE C, GIORGIA P, et al. Evolution of hyphenated techniques for mineral oil analysis in food[J]. Journal of Separation Science, 2021, 44（1）: 464-482.
[12] JAEN J, DOMENO C, NERIN C, et al. Development of an analytical method for the determination of mineral oil aromatic hydrocarbons （MOAH） from printing inks in food packaging[J]. Food Chemistry, 2022, 397: 133745.
[13] GREGORY B, CHIARA C, NICOLA S, et al. Quantification and characterization of mineral oil in fish feed by liquid chromatography-gas chromatography-flame ionization detector and liquid chromatography-comprehensive multidimensional gas chromatography-time-of-flight mass spectrometer/flame ionization detector[J]. Journal of Chromatography A, 2022, 1 677: 463208.
[14] GREGORY B, LAURA B, GIORGIA P, et al. Validation of the liquid chromatography-comprehensive multidimensional gas chromatography-time-of-flight mass spectrometer/flame ionization detector platform for mineral oil analysis exploiting interlaboratory comparison data[J]. Green Analytical Chemistry, 2023, 4: 100047.
[15] RUIZ J L H, LIEBANAS J A, VIDAL J L M, et al. Offline solid-phase extraction and separation of mineral oil saturated hydrocarbons and mineral oil aromatic hydrocarbons in edible oils, and analysis via GC with a flame ionization detector[J]. Foods, 2021, 10（9）: 2 026.
[16] 陈燕芬, 曾莹, 吴泽春, 等. 全二维气相色谱—飞行时间质谱测定婴幼儿配方奶粉中的矿物油[J]. 食品安全质量检测学报, 2020, 11（7）: 2 066-2 074. CHEN Y F, ZENG Y, WU Z C, et al. Determination of mineral oil in infant formula by comprehensive two-dimensional gas chromatography with time of flight mass spectrometry[J]. Journal of Food Safety and Quality, 2020, 11（7）: 2 066-2 074.
[17] BAUWENS G, PANTO S, PURCARO G, et al. Mineral oil saturated and aromatic hydrocarbons quantification: Mono- and two-dimensional approaches[J]. Journal of Chromatography A, 2021, 1 643: 462044.
[18] MARIOSIMONE Z, TANIA M, PETER Q, et al. Use of a low-cost, lab-made Y-interface for liquid-gas chromatography coupling for the analysis of mineral oils in food samplel[J]. Journal of Chromatography A, 2021, 1 648: 462191.
[19] 柯润辉, 杨春艳, 胡雪, 等. 固相萃取—气相色谱法定量分析橄榄油中饱和烃矿物油和芳香烃矿物油[J]. 分析化学, 2018, 46（10）: 1 677-1 684. KE R H, YANG C Y, HU X, et al. Off-line solid phase extraction combined with gas chromatography-flame ionization detection method for determination of mineral oil saturated and aromatic hydrocarbons in olive oils[J]. Chinese Journal of Analytical Chemistry, 2018, 46（10）: 1 677-1 684.
[20] MORET S, GROB K, CONTE L S, et al. On-line high-performance liquid chromatography-solvent evaporation-high-performance liquid chromatography-capillary gas chromatography-flame ionisation detec-tion for the analysis of mineral oil polyaromatic hydrocarbons in fatty foods[J]. Journal of Chromatography A, 1996, 750（1/2）: 361-368.
[21] BARP L, PURCARO G, MORET S, et al. A high-sample-throughput LC-GC method for mineral oil determination[J]. Journal of Separation Science, 2013, 36（18）: 3 135-3 139.
[22] PURCARO G, ZOCCALI M, TRANCHIDA P Q, et al. Comparison of two different multidimensional liquid-gas chromatography inter-faces for determination of mineral oil saturated hydrocarbons in foodstuffs[J]. Analytical and Bioanalytical Chemistry, 2013, 405（2/3）: 1 077-1 084.
[23] ALASDAIR M. Modern mineral oil hydrocarbon analysis[J]. LC GC North America, 2023, 41（7）: 274-276.
[24] MORET S, BARP L, GROB K, et al. Optimised off-line SPE-GC-FID method for the determination of mineral oil saturated hydrocar-bons （MOSH） in vegetable oils[J]. Food Chemistry, 2011, 129（4）: 1 898-1 903.
[25] MORET S, BARP L, PURCARO G, et al. Rapid and sensitive solid phase extraction-large volume injection-gas chromatography for the analysis of mineral oil saturated and aromatic hydrocarbons in card-board and dried foods[J]. Journal of Chromatography A, 2012, 1 243: 1-5.
[26] FISELIER K, GRUNDBOCK F, SCHON K, et al. Development of a manual method for the determination of mineral oil in foods and pa-perboard[J]. Journal of Chromatography A, 2013, 1 271（1）: 192-200.
[27] International Organization for Standardization. Animal and vegetable fats and oils determination of aliphatic hydrocarbons in vegetable oils: ISO 17780: 2015（E） [S]. Switzerland: ISO Copyright Office, 2015: 1-29.
[28] 刘玲玲, 张贞霞, 李冰宁, 等. 离线SPE-LVI-GC-FID法分析婴儿配方奶粉中的饱和烃类矿物油[J]. 食品科学, 2017, 38（22）: 303-308. LIU L L, ZHANG Z X, LI B N, et al. Off-line solid phase extraction-large volume injection-gas chromatography-flame ionization detection （SPE-LVI-GC-FID） for the analysis of mineral oil saturated hydrocarbons （MOSH） in infant formula[J]. Food Science, 2017, 38（22）: 303-308.
[29] 张洋, 李晓娟, 汪春明, 等. 离线固相萃取—气相色谱法定量分析巧克力中饱和烃类矿物油[J]. 食品与发酵工业, 2021, 47（21）: 253-258. ZHANG Y, LI X J, WANG C M, et al. Off-line solid phase extraction-gas chromatography-flame ionization detection of mineral oil saturated hydrocarbons in chocolate[J]. Food and Fermentation Industries, 2021, 47（21）: 253-258.

Download

Share

COinS
 
 

To view the content in your browser, please download Adobe Reader or, alternately,
you may Download the file to your hard drive.

NOTE: The latest versions of Adobe Reader do not support viewing PDF files within Firefox on Mac OS and if you are using a modern (Intel) Mac, there is no official plugin for viewing PDF files within the browser window.