超高效液相色谱-串联质谱法测定食品中4种罂粟壳生物碱

Simultaneous Determination of Four Opium Poppy Husk Alkaloids in Residues of Foods Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定食品中可卡因、可待因、吗啡、盐酸罂粟碱的检测方法.样品经氨化甲醇提取,采用Capcell Pak C18(250 mm×2.0 mm,MGII 5 μm)色谱柱,以色谱纯乙腈为流动相A,以20 mmol/L乙酸铵和0.1%甲酸缓冲液为流动相B,进行梯度洗脱.在优选条件下,可待因、吗啡方法线性范围为5.0~50.0 μg/L,可卡因、盐酸罂粟碱的方法线性范围为1.0~20.0 μg/L,相关系数均大于0.999,方法检出限在0.1~0.8 μg/kg之间,平均回收率为76.0%~111.2%,相对标准偏差RSD低于10%.

     

    Abstract: A method of ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of four opium poppy husk alkaloids (i. e., cocaine, codeine, morphine and papaverine hydrochloride) in the residues of foods. The samples were extracted by methanol (containing 5 % ammonia acetate) followed by analyzed on a UPLC-MS/MS system (AJS ESI positive mode) equipped with a Capcell Pak C18(250 mm×2.0 mm, MGII 5 μm) column with the mobile phase of acetonitrile and aqueous solution of ammonium acetate (20 mmol/L) containing formic acid (0.1 %) as the additive. Under optimized conditions, the linear range for codeine and morphine were 5.0~50.0 μg/L, and those for cocaine and papaverine were 1.0~20.0 μg/L, with relative coefficients above 0.999. The limits of detection for the method was in the range of 0.1~0.8 μg/kg, and average spiking recovery was in the range of 76.0%~111.2 % with RSDs below 10%.

     

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