摘要
本文旨在建立同时测定饲料中没食子酸丙酯(PG)、特丁基对苯二酚(TBHQ)、乙氧基喹啉(EQ)、丁基羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)5 种合成类抗氧化剂含量的高效液相色谱法。试样经超声波辅助乙腈直接提取,提取液经有机相针式滤器过滤净化后,采用十八烷基键合相(C_(18))柱为色谱柱 (长 150 mm×内径 4.6 mm,粒径 5 μm),乙腈-2%乙酸溶液(65 + 35,V_(1)+V_(2))为流动相,流速为 0.5 m L/min,检测波长为 280 nm,柱温为 20 ~ 30℃。在此实验条件下,PG 在质量浓度 0.50 ~ 25.00 μg/mL,TBHQ、EQ、BHA 和 BHT 在质量浓度 1.00 ~ 50.00 μg/mL 内均与峰面积呈良好的线性关系(相关系数 r^(2 )> 0.999);PG、TBHQ、EQ、BHA 和 BHT 的检出限分别为 1.8、1.9、2.0、1.9、5.0 mg/kg,定量限分别为 8.8、8.6、8.9、8.7、10.0 mg/kg;PG、TBHQ、EQ、BHA 和 BHT 加标回收率 (RSD,n=5)分别为 76.2% ~ 98.8%(RSD 1.1% ~ 9.5%),77.2% ~ 97.8%(RSD 0.9% ~ 4.3%),77.3% ~ 98.0%(RSD 0.7% ~ 6.9%),76.7% ~ 95.8%(RSD 1.1% ~ 6.2%)和 75.3% ~ 95.8%(RSD 0.9% ~ 7.1%)。本法操作简便、快速、结果准确,适用于同时测定饲料中 5 种合成类抗氧化剂含量。
An HPLC method for simultaneous dete rmination of propyl gallate (PG),tert buty hydroquinone (TBHQ),ethoxyquin (EQ),butyl hydroxyanisole (BHA) and dibutyl hydroxytoluene (BHT) in feeds was developed.Five synthetic antioxidants in samples were extracted with acetonitrile by ultrasound extraction,purified by the organic phase needle type filter and then separation was carried out with C_(18)column(150 mm × 4.6 mm,5 μm) with the mobile phase of acetonitrile - 2% acetic acid solution (65 + 35,V_(1)+V_(2))at a flow rate of 0.5 mL/min,the detection wavelength was 280 nm,and the column temperature was 20 ~ 30 ℃Under above experimental conditions,the good linear relationships were obtained within the ranges of 0.50 ~25.00 μg/mL for PG,and 1.00 ~ 50.00 μg/mL for TBHQ,EQ,BHA and BHT (r~2> 0.999).The detection limits of PG,TBHQ,EQ,BHA and BHT were 1.8,1.9,2.0,1.9 mg/kg and 5.0 mg/kg respectively,and the quantitative limits were 8.8,8.6,8.9,8.7 mg/kg and 10.0 mg/kg respectively;The spiked recoveries (RSD,n=5) of PG,TBHQ,EQ,BHA and BHT were 76.2% ~ 98.8% (RSD 1.1% ~ 9.5%),77.2% ~ 97.8% (RSD 0.9% ~4.3%),77.3% ~ 98.0%(RSD 0.7% ~ 6.9%),76.7% ~ 95.8%(RSD 1.1% ~ 6.2%) and 75.3% ~ 95.8%(RSD0.9% ~ 7.1% ) respectively.The method was simple,rapid and accurate.It is suitable for the simultaneous determination of five synthetic antioxidants in feeds.
作者
商军
张浩然
田恺
华贤辉
徐汀
SHANG Jun;ZHANG Haoran;TIAN Kai;HUA Xianhui;XU Ting(Shanghai Institute for Veterinary Drug&Feeds control,Shanghai 201103,China)
出处
《中国饲料》
北大核心
2022年第17期80-88,共9页
China Feed
