摘要
以硅酸镁、硅胶、硅藻土、硫酸钙为原料,加入乙醇研磨成匀浆,干燥,填充于聚丙烯柱管中,制备成新型固相萃取小柱。样品经果胶酶酶解,乙腈提取,固相萃取净化,以C18色谱柱(100 mm×2.1 mm,1.8μm)为分离色谱柱进行定性、定量分析。流动相为0.8%(体积分数)四氢呋喃水溶液,流速为0.5 mL/min,以276 nm波长进行检测。考察了果胶酶对萃取效果的影响、固相萃取小柱的净化效果及最佳色谱分析条件。在0.1~10 mg/L范围内,展青霉素峰高与质量浓度呈良好的线性关系,相关系数(R^2)为1,方法检出限为10.22μg/kg,样品的加标回收率为86.58%~94.84%,相对标准偏差(RSD)为1.45%~2.28%。实验结果表明,自制固相萃取小柱净化效果好,超高效液相色谱分离效能高,样品测定操作方法简单,结果准确,对水果制品的质量安全控制具有重要的意义。
With magnesium silicate,silica gel,diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate,drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase,extracted by acetonitrile and purified by solid phase extraction. The target com-pounds were separated on a C18 column （100 mmx2. 1 mm,1. 8p m） ,using 0. 8% （ v/v） tetra- hydrofuran solution as mobile phase with a flow rate of 0. 5 mL^min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0. 1 to 10 mg/L with the correlation coefficient （ R^2） of 1. The limit of detection for this method was 10. 22 μg/kg. The spiked recoveries of samples were 86. 58% - 94.84% with the relative standard deviations （RSDs） of 1.45% -2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency,and the UPLC had a high separation efficiency. The method is simple,accurate and of great significance for the quality and safety control of fruit products.
出处
《色谱》
CAS
CSCD
北大核心
2017年第11期1160-1164,共5页
Chinese Journal of Chromatography
基金
黑龙江省教育厅基本业务专项(135209221
135109206)~~
关键词
固相萃取
超高效液相色谱
展青霉素
水果制品
solid phase extraction （SPE）
ultra performance liquid chromatography （UPLC）
patulin （PAT）
fruit products
