HPLC Determination of Residual Amount of Extracts of Poppy Shell in Soup Blend with Sample Pretreatment by Solid Phase Extraction
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10 μL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0.05~50 mg·L-1,检出限(3S/N)依次为0.010,0.010,0.015 mg·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%。
Abstract
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%.
中图分类号 O652.63
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收稿日期 2011/1/11
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备注谷岩(1975-),女,辽宁沈阳人,高级工程师,硕士研究生,主要研究方向为色谱及质谱分析。
引用该论文: GU Yan,LIU Guang-fu,ZHANG Yuan,QIU Zhao-jun. HPLC Determination of Residual Amount of Extracts of Poppy Shell in Soup Blend with Sample Pretreatment by Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(12): 1411~1413
谷岩,刘广福,张元,邱兆军. 固相萃取-高效液相色谱法测定汤料中罂粟壳提取物残留量[J]. 理化检验-化学分册, 2011, 47(12): 1411~1413
被引情况:
【1】沈平,谢朝梅,谢燕湘, "气相色谱-质谱法测定食品中罂粟壳提取物的残留量",理化检验-化学分册 52, 48-51(2016)
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【4】闫瑾,赵美萍,李元宗,等.罂粟碱检测方法研究进展[J].化学进展杂志, 2005,22(5):140-147.
【5】POPA D S, OPREAN R, CUREA E, et al. TLC-UV densitomet ric and GC-MSD methods for simultaneous quantification of morphine and codeine in poppy capsules[J]. Journal of Pharmaceutical and Biomedical Analysis ,1998,18:645-650.
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【7】LIU Song-yun, WOO S O, MICHAEL J H , et al. LC and LC-MS-MS analysis of undeclared codeine in antiasthmatic Chinese propriet ry medicine[J]. Journal of Pharmaceutical and Biomedical Analysis, 2000,22:481-486.
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【9】张虹,廖文娟,蔡增轩,等.液质联用法检测罂粟壳食物中生物碱的残留[J].分析与检测杂志, 2006,31(12):93-97.
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【11】黄卫平.食品中罂粟壳残留检测方法[J].中国公共卫生, 2002,18(1):111-113.
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