气相色谱-质谱法测定食品中的3-乙酰基-2,5-二甲基噻吩

Determination of 3-acetyl-2,5-dimethyl thiophene in food by gas chromatography-mass spectrometry

针对含油脂食品、不含油脂食品分别建立了有效的前处理方法,利用气相色谱-质谱技术,建立了一种简便高效、高灵敏度的检测食品中3-乙酰基-2,5-二甲基噻吩的定性定量分析方法。含油脂食品经甲醇提取后冷冻过滤、不含油脂食品经正己烷提取后离心,以气相色谱-质谱为检测手段,外标法定量。研究结果显示,3-乙酰基-2,5-二甲基噻吩在0.005μg/mL^1μg/mL浓度范围内曲线线性良好,相关系数为0.9999;在不同基质及不同加标浓度下,加标回收率为86.6%~104.6%,相对标准偏差(RSD_S,n=6)为0.9%~1.9%;3-乙酰基-2,5-二甲基噻吩在不同基质中的检出限均可达到0.01mg/kg,定量限达到0.03mg/kg。该方法前处理操作简便、技术难度低,准确度和灵敏度高,抗干扰能力强,定性定量准确并快速的测定出食品中3-乙酰基-2,5-二甲基噻吩的残留量。

A simple,efficient and high sensitive qualitative and quantitative method for the determination of 3-acetyl-2,5-dimethyl thiophene in food was established by gas chromatography-mass spectrometry.Food containing oil was extracted by methanol and then frozen and filtered,while food without oil was extracted by n-hexane and centrifuged.The results showed that the curve of 3-acetyl-2,5-dimethylthiophene was linear in the concentration range of 0.005μg/mL^1μg/mL,and the correlation coefficient was 0.9999.Under different substrates and different additive concentrations,the recoveries were 86.6%~104.6%,and the relative standard deviation(RSDS,n=6)was 0.9%~1.9%.The detection limit of 3-acetyl-2,5-dimethyl thiophene in different substrates can reach 0.01 mg/kg,and the quantitative limit can reach 0.03 mg/kg.This method is simple to operate,less technical problems,high accuracy and sensitivity,strong anti-interference ability,accurate in qualitative and quantitative detection and rapid determination of food residues of 3-acetyl-2,5-dimethyl thiophene.