关键词: Bakery products Cholesterol GC-FID Method validation Tocopherol Trimethylsilyl derivatization

来  源:   DOI:10.1016/j.heliyon.2024.e30596   PDF(Pubmed)

Abstract:
Cholesterol analysis by derivatization technique is a time consuming, costly, and complex process while analyzing cholesterol without derivation is a simple, and quick method.Researchers analyzed cholesterol using both derivatization and non-derivatization techniques successfully. The objective of this study was to investigate the effect of derivatization in cholesterol analysis particularly on bakery goods.The retention time of non-derivatized cholesterol (11.62 min) and non-derivatized α-tocopherol standard (11.60 min) was very close in HP-5 capillary GC column andthey eluted together while injected as mixed standard. As a result, cholesterol content determined by non-derivatized technique could be overestimated due to the presence of α-tocopherol inbakery products. The peak resolution (Rs) between derivatized cholesterol and derivatized α-tocopherol standard using the appliedgradient GC condition was 3.1 which is well separated (>1.5) based on AOAC guidelines. The derivatized gas chromatographic cholesterol analysis method was verified by limit of detection (LOD; 0.03 mg/100 g), limit of quantification (LOQ; 0.08 mg/100 g), linearity (R2; 0.999),precision (repeatability: relative standard deviation (RSD) 1.5 %; reproducibility: RSD 1.9 %), and accuracy (102.1 % recovery). The verified cholesterol analysis method was subsequently applied to determine cholesterol content in selected bakery items, yielding a range of 2.76 ± 0.06 mg/100 g (chrysanthemum bread) to 114.26 ± 4.72 mg/100 g (castella).
摘要:
通过衍生化技术进行胆固醇分析是耗时的,昂贵的,和复杂的过程,而不推导分析胆固醇是一个简单的,和快速的方法。研究人员使用衍生和非衍生技术成功地分析了胆固醇。这项研究的目的是研究衍生化在胆固醇分析中的作用,尤其是对面包店的影响。非衍生化胆固醇(11.62分钟)和非衍生化α-生育酚标准品(11.60分钟)在HP-5毛细管GC色谱柱中的保留时间非常接近,并且作为混合标准品注射时它们一起洗脱。因此,由于存在α-生育酚烘烤产品,通过非衍生技术确定的胆固醇含量可能被高估。使用所应用的梯度GC条件,衍生化胆固醇和衍生化α-生育酚标准品之间的峰分辨率(Rs)为3.1,基于AOAC指南,分离良好(>1.5)。通过检测限(LOD;0.03mg/100g)验证了衍生气相色谱胆固醇分析方法,定量限(LOQ;0.08mg/100g),线性(R2;0.999),精密度(重复性:相对标准偏差(RSD)1.5%;重复性:RSD1.9%),和准确性(102.1%的回收率)。随后将经过验证的胆固醇分析方法用于确定选定的烘焙项目中的胆固醇含量,产生范围为2.76±0.06mg/100g(菊花面包)至114.26±4.72mg/100g(城堡)。
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