盐水鹅中5种罂粟壳生物碱的固相萃取-液相色谱串联质谱同时测定法  

Simultaneous determination of five poppy husk alkaloidsin salted gooseby solid-phase extraction-liquid chromatography-tandem mass spectrometry

作　　者：朱文杰[1] ZHU Wen-jie(Test Department,Hanjiang Center for Disease Control and Prevention,Yangzhou Jiangsu,225000,China)

机构地区：[1]扬州市邗江区疾病预防控制中心检验科,江苏扬州225000

出　　处：《职业与健康》2022年第20期2766-2770,共5页Occupation and Health

摘　　要：目的建立盐水鹅中5种罂粟壳生物碱的固相萃取-液相色谱串联质谱分析方法。方法样品经乙腈/水(90∶10 V/V,含0.2%甲酸)提取,用混合型阳离子交换固相萃取小柱净化。以乙腈和水(含0.1%甲酸)为流动相,采用梯度洗脱方式在ACQUITY UPLC BEH C(100 mm×2.1 mm,1.7μm)色谱柱上进行分离,以电喷雾多反应监测正离子模式进行检测。结果吗啡和可待因的检出限均为0.017μg/kg,蒂巴因、罂粟碱和那可丁的检出限均为0.003μg/kg。吗啡和可待因在0.05~25.00μg/L范围内,蒂巴因、罂粟碱和那可丁在0.01~5.00μg/L范围内线性关系均良好(r>0.999),5种生物碱的准确度(以回收率表示)在92.33%~106.42%之间,精密度(以相对标准偏差表示)在2.42%~6.12%之间(n=6)。结论该法快速高效、重现性好,可用于盐水鹅中5种罂粟壳生物碱的测定。Objective To develop a method for the determination of five poppy husk alkaloids in salted goose by solid-phase extraction(SPE)and liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The sample was extracted with acidified acetonitrile/water(90∶10V/V,containing 0.2%formic acid),and purified with mixed-mode cation exchange(MCX)SPE column.The LC separation was performed on a ACQUITY UPLC BEH C(100 mm×2.1 mm,1.7μm)using acetonitrile and water(0.1%formic acid)as the mobile phase with a gradient elution program.The determinationwas applied by electrospray ionization with multiple reaction monitoring in positive ion mode.Results The limits of detection for morphine and codeine were both 0.017μg/kg,and that for tibain,papaverine and nacodin were all 0.003μg/kg.The calibration curves showed good linearity between 0.05-25.00μg/L for morphine and codeine,0.01-5.00μg/L for tibain,papaverine and nacodin(r>0.999).The accuracy(expressed in terms of recovery)for five alkaloidswas 92.33%-106.42%,and precision(expressed in relative standard deviation)was 2.42%-6.12%(n=6).Conclusion The method is rapid,highly efficient andreproducible,which can be used for the determination of the five poppy husk alkaloids in salted goose.

关 键 词：液相色谱串联质谱法 盐水鹅 罂粟壳生物碱 

分 类 号：R115[医药卫生—公共卫生与预防医学]