摘要
提出了高效液相色谱法测定汤料中罂粟壳提取物吗啡、可待因和罂粟碱残留量的方法。样品用乙醚萃取,经离心分离,取上清液通过固相萃取柱纯化。流出液经过滤后,取10μL进样,在Zorbax SB C18色谱柱上进行分离,以不同比例混合的乙酸铵溶液和甲醇作为流动相进行梯度淋洗。吗啡、可待因和罂粟碱的线性范围均为0.05～50mg.L-1,检出限(3S/N)依次为0.010,0.010,0.015mg.kg-1。以空白肉汤实样为基体做加标回收试验,测得回收率依次在94.0%～97.1%,89.0%～94.9%,91.0%～93.0%之间,相对标准偏差(n=6)均小于5.5%。
A method for determination of the extracts of poppy shell,i.e.morphine,codeine and papaverine,in soup blend was proposed.The sample was extracted with ether and after centrifugation,the supernatant was purified by passing through the solid phase extraction column.The eluent from the column was filtered and used for HPLC analysis.Ten μL of the eluent were introduced into the instrument and separated on the Zorbox SB C18 chromatographic column,using a mixed solution of ammonium acetate and methanol with different proportions as mobile phase in gradient elution.Ranges of linearity found were same between 0.05-50 mg·L-1,with detection limits（3S/N） of 0.010 mg·kg-1（for morphine）,0.010 mg·kg-1（for codeine） and 0.015 mg·kg-1（for papaverine） respectively.Recovery was tested by addition of standards to blank sample of soup blend,giving values of recovery in the range of 94.0%-97.1%（for morphine）,89.0%-94.9%（for codeine） and 91.0%-93.0%（for papaverine） with values of RSD′s（n=6） less than 5.5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第12期1411-1413,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
