超高效液相色谱-电喷雾电离串联质谱法测定农产品中的井冈霉素  

Determination of validamycin residues in agricultural products by ultra high performance liquid chromatography-electrospray ionization-tandem mass spectrometry

作　　者：肖桂英 池连学 于璐莹 李帅 王丹 孙燕华 张禧庆 Xiao Guiying;Chi Lianxue;Yu Luying;Li Shuai;Wang Dan;Sun Yanhua;Zhang Xiqing(Shandong Jienuo Testing Service Co.,Ltd,Yantai 265231,China;Longda Foodstuff Group Co.,Ltd.,Yantai 265231,China;Laiyang Longwangzhuang Animal Husbandry and Veterinary Station,Yantai 265209,China)

机构地区：[1]山东杰诺检测服务有限公司,烟台265231 [2]龙大食品集团有限公司,烟台265231 [3]莱阳市龙旺庄畜牧兽医站,烟台265209

出　　处：《分析仪器》2023年第4期43-48,共6页Analytical Instrumentation

摘　　要：建立了超高效液相色谱-电喷雾电离串联质谱技术测定农产品中井冈霉素残留的分析方法。样品用甲醇-10 mM乙酸铵水溶液(7/3,v/v,pH5.5)提取,经硅藻土结合混合型阳离子交换柱(mixed cation exchange column,PCX)净化,采用亲水作用色谱(hydrophilic interaction chromatography,HILIC)梯度洗脱分离,电喷雾电离源(electrospray ionization,ESI),多反应监测(multiple reaction monitoring,MRM)扫描。井冈霉素在1~40μg/L线性范围内,线性关系良好(r>0.995),方法定量限10μg/kg,在1倍、2和10倍定量限3个浓度添加水平下,果蔬类添加回收率在85.06%~94.73%之间,重复性精密度在4.80%~5.92%之间;粮谷类添加回收率在79.26%~89.12%之间,重复性精密度在4.88%~6.01%之间。该方法灵敏度高、准确度高、重现性好,适用于果蔬、粮谷等多种农产品井冈霉素的检测。The sample was extracted with methanol-10 mM ammonium acetate aqueous solution(7:3,v/v,adjusted pH 5.5 with glacial acetic acid),purified with diatomite combined with mixed strong cation exchange column PCX,separated by gradient elution with HILIC chromatographic column,scanned by electrospray ionization(ESI)and multiple reaction monitoring(MRM).The calibration curves of validamycin were linear in the range of 1—40μg/L with the correlation coefficients more than 0.995.The determination limit of the method was 10µg/kg.At the three concentration addition levels of 1LOQ,2LOQ and 10LOQ,the addition recovery of fruit and vegetable was within 85.06%—94.73%,and the repeatability precision was within 4.80%—5.92%;the addition recovery of grain was within 73.63%—91.40%,and the repeatability precision was within 3.72%—6.09%.The method has high sensitivity,accuracy and reproducibility,and is suitable for the detection of validamycin in various agricultural products.

关 键 词：超高效液相色谱-电喷雾电离串联质谱 井冈霉素 农产品 硅藻土 混合型阳离子交换柱(PCX) 亲水作用色谱(HILIC) 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]