QuEChERS前处理高效液相色谱法同时测定酵母产品中7种合成酚类抗氧化剂

Simultaneous determination of 7 synthetic phenolic antioxidants in yeast products using QuEChERS sample preparation and high performance liquid chromatography

建立了QuEChERS-HPLC同时定量测定酵母中的没食子酸(GA)、没食子酸丙酯(PG)、叔丁基对苯二酚(TBHQ)、没食子酸异戊酯(IAG)、没食子酸辛酯(OG)、没食子酸十二酯(DG)和二丁基羟基甲苯(BHT)7种合成酚类抗氧化剂(SPAs)的分析方法。样品用乙腈提取,经PCX粉净化,以JADE-PAK C18色谱柱(4.6 mm×150mm,5μm)分离,采用1%乙酸水溶液和甲醇为流动相梯度洗脱,二极管阵列检测器(DAD)检测,结合保留时间和紫外光谱进行定性分析,定量波长280 nm。7种合成酚类抗氧化剂(SPAs)在各自的范围内相关系数(r2)均大于0.994,定量限(LOD,S/N=10)为1~10 mg/kg;3个加标水平(1、2、10倍定量限)下,活性干酵母和酵母抽提物中回收率分别在79.7%~102.4%和79.3%~107.4%,相对标准偏差(RSD)分别在2.5%~8.7%和2.7%~9.6%。该方法准确快速、灵敏度高,适用于酵母产品中7种合成酚类抗氧化剂(SPAs)的同时测定。

A method was （SPAs） , including gallic acid（ developed for the simultaneous determination of 7 synthetic phenolic antioxidants GA）, propyl gallate （ PG）, tertiary butylhydroquinone （ TBHQ ）, isoamyl gallate （ IAG ） , oetyl gallate（OG） ,dodecyl gallate（DG） and butylated hydroxytoluene（ BHT）, in yeast products by using high per- formance liquid chromatographic （HPLC） method. The yeast products was extracted with acetonitrile and then cleaned up by PCX. The separation of analytes was performed on a JADE-PAK Cls column （4.6 mm × 150 mm, 5 μm） by gradient elution using 1% aqueous acetic acid solution and methanol as mobile phase. The sample was sepa- rated and detected with photodiode array detector （ DAD）. The qualification analysis was performed by using retention time and UV spectrum, and the quantification affalysis was based on the detection wavelength of 280 nm. The calibra- tion curves showed good linearity for seven synthetic phenolic antioxidants （SPAs） , and the correlation coefficients （ r^2） were higher than 0. 994. The limits of quantification （ LOQs, S/N 〉 10） were in the range of 1-10 mg/kg. The average recoveries were in the range of 79.7 % - 102.4 % and 79.3 % - 107.4 % for seven antioxidants respective- ly in active dry yeast and yeast extract, with the relative standard deviations （RSDs） of 2.5 % - 8.7 % and 2.7 % -9.6 % at the spiked levels of 1,2,10 LOQ. The method is accurate, rapid and sensitive, and suitable for monito- ring of seven synthetic phenolic antioxidants （SPAs） in yeast products.