超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量  

Determination of Morphine,Codeine,Thebaine,Narcotine and Papaverine Residues in Seasonings by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张哲 张莹[1] 赵桐 赵灵智 沈晶萍 王世琨 李思圆 ZHANG Zhe;ZHANG Ying;ZHAO Tong;ZHAO Ling-zhi;SHEN Jing-ping;WANG Shi-kun;LI Si-yuan(College of Life Sciences,Jilin Agricultural University,Changchun 130118,China)

机构地区：[1]吉林农业大学生命科学学院,长春130118

出　　处：《中国调味品》2023年第3期161-169,共9页China Condiment

基　　金：吉林省自然科学基金学科布局项目(20210101370JC);吉林省大学生创新创业训练计划项目(202010193110)。

摘　　要：目的:建立超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量的分析方法。方法:样品用水分散、乙腈超声提取,经盐析、低温高速离心分层后,样液于40℃水浴氮吹近干,用10%乙腈溶液(含0.1%甲酸)溶解残渣,再经低温高速离心、过膜上机测定;以Kinetex^(■)2.6μm Biphenyl 100Å色谱柱(100 mm×3.0 mm)分离,0.1%甲酸-水和0.1%甲酸-甲醇为流动相进行梯度洗脱,电喷雾电离(ESI),正离子模式,多反应监测(MRM)下检测,吗啡、可待因用内标法定量,蒂巴因、那可丁、罂粟碱用外标法定量。结果:吗啡、可待因在0.5~20.0 ng/mL,蒂巴因在0.10~4.0 ng/mL,那可丁、罂粟碱在0.05~2.0 ng/mL范围内均有良好的线性关系,相关系数r均大于0.998。吗啡、可待因的方法检出限为1.0μg/kg,蒂巴因的方法检出限为0.2μg/kg,那可丁、罂粟碱的方法检出限为0.1μg/kg。5种生物碱的加标回收率在75.2%~117.3%之间,相对标准偏差均小于15%。结论:该方法操作简单,具有较高的灵敏度、准确度和重现性,可用于调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱的痕量分析。Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of morphine,codeine,thebaine,narcotine and papaverine residues in seasonings.Method:The sample is dispersed with water and extracted with acetonitrile by ultrasonic extraction method.After salting out and low-temperature high-speed centrifugation and layering,the sample solution is blown to nearly dry with nitrogen in water bath at 40℃.The residues are dissolved with 10%acetonitrile solution(containing 0.1%formic acid),centrifuged at low temperature with high speed,filtered through membranes and detected.The samples are separated by Kinetex^(■)2.6μm Biphenyl 100Åchromatographic column(100 mm×3.0 mm)with 0.1%formic acid-water and 0.1%formic acid-methanol as the mobile phases for gradient elution.Electrospray ionization(ESI)is used to detect under positive ion mode multi-reaction monitoring(MRM).Morphine and codeine are quantified with the internal standard method,and thebaine,narcotine and papaverine are quantified with the external standard method.Results:Morphine and codeine have good linear relationships in the range of 0.5~20.0 ng/mL,thebaine has a good linear relationship in the range of 0.10~4.0 ng/mL,narcotine and papaverine have good linear relationships in the range of 0.05~2.0 ng/mL,and the correlation coefficient r is greater than 0.998.The method detection limit of morphine and codeine is 1.0μg/kg,the method detection limit of thebaine is 0.2μg/kg,and the method detection limit of narcotine and papaverine is 0.1μg/kg.The spiked recovery rates of the five alkaloids are between 75.2%and 117.3%,and the relative standard deviations are all less than 15%.Conclusion:The method is simple to operate,has high sensitivity,accuracy and reproducibility,and can be used for the trace analysis of morphine,codeine,thebaine,narcotine and papaverine in seasonings.

关 键 词：调味料 吗啡 可待因 蒂巴因 那可丁 罂粟碱 超高效液相色谱-串联质谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学]