GC-MS/MS法检测恒顺降脂醋胶囊中的5种脂肪酸

Determination of five fatty acids in Heng Shun vinegar capsule by GC-MS/MS

该研究建立了恒顺降脂醋胶囊中5种脂肪酸的硅烷化衍生-气相色谱-三重四级杆质谱(GC-MS/MS)测定方法。样品采用氢氧化钾甲醇溶液皂化,经稀盐酸中和剩余的碱后,待测组分用正己烷提取。取50μL正己烷层,加入吡啶、硅烷化试剂衍生。经过DB-5MS毛细管气相色谱柱分离,在多反应离子监测模式下(MRM)进行检测,外标法定量。各目标物在0.125~16.0 mg/kg(油酸)、0.501~65.6 mg/kg(亚油酸)、0.440~56.0 mg/kg(α-亚麻酸)、0.750~96.0 mg/kg(γ-亚麻酸)、0.141~26.0 mg/kg(共轭亚油酸)范围内线性关系良好,相关系数(R^2)均>0.992。油酸、亚油酸、α-亚麻酸、γ-亚麻酸、共轭亚油酸的定量限(信噪比S/N=10)分别为0.17%、0.57%、0.50%、0.82%、0.20%;检出限(S/N=3)分别为0.052%、0.17%、0.15%、0.25%、0.061%。5种脂肪酸的回收率为75.0%~103.8%,相对标准偏差(RSD)为2.3%~6.6%。该方法的灵敏度、准确度和精密度均符合相关的技术要求,适用于醋胶囊中脂肪酸含量的检测。

A new method for determination of five kinds of fatty acids in HengShun vinegar capsule by silylation derivatization-gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)was developed.The sample was saponified with the mixture solution of potassium hydrate and methanol,and then the redundant base was neutralized by dilute hydrochloric acid,and the component to be tested was extracted with n-hexane.50μl n-hexane phase was transferred into centrifuge tube and derived with pyridine and silylating reagent.The sample was separated by DB-5MS capillary gas chromatography column,detected under multiple reaction monitoring(MRM)and quantified by external standard method.The linear relationships in the range of 0.125-16.0 mg/kg(oleic acid),0.501-65.6 mg/kg(inoleic acid),0.440-56.0 mg/kg(α-linolenic acid),0.750-96.0 mg/kg(γ-linolenic acid),0.141-26.0 mg/kg(conjugated linoleic acid)were good,and the correlation coefficient(R2)was greater than 0.992.The limits of quantitation(the signal to noise ratio was 10)of oleic acid,inoleic acid,α-linolenic acid,γ-linolenic acid and conjugated linoleic acid were 0.17%,0.57%,0.50%,0.82%,0.20%,respectively,and the limits of detection(the signal to noise ratio was 3)were 0.052%,0.17%,0.15%,0.25%,0.061%,respectively.The recovery rate of the five fatty acids was in the range of 75.0%-103.8%,and the relative standard deviation(RSD)was in the range of 2.3%-6.6%.The sensitivity,accuracy and precision of the method were in line with relevant technical requirements and suitable for the detection of fatty acid content in vinegar capsules.