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分散固相萃取结合通过式固相萃取净化-超高效液相色谱-串联质谱法测定火锅底料中5种罂粟壳生物碱
其他题名Determination of 5Alkaloids fromPericarpium Papaveris in Hot Pot Soup Base by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Dispersive and Pass-through Solid-phase Extraction
吴琼; 扈明洁; 江海; 励炯; 邱红钰; 李玮
来源期刊分析科学学报
ISSN1006-6144
出版年2021
卷号37期号:2页码:1006-6144
中文摘要本文建立了火锅底料中5种罂粟壳生物碱的分散固相萃取,结合通过式固相萃取净化-超高效液相色谱-串联质谱法的检测方法。样品先用80%的乙腈水溶液提取,提取液经Oasis PRiME HLB固相萃取柱进行初步净化。净化后的溶液加入由无水Na_2SO_4、十八烷基键合硅胶吸附剂(C_(18)-N)及氨丙基乙二胺吸附剂(NH2-PSA)组成的净化剂进一步的净化。净化溶液用Waters CORTECS UPLC HILIC柱(100mm*2.1mm, 1.6mum)进行分离,流动相为乙腈和含0.1%甲酸的10mmol/L甲酸铵溶液,梯度洗脱,并采用电喷雾电离正离子模式,以多反应监测(MRM)定性定量分析目标化合物。考察了净化剂中无水Na_2SO_4、C_(18)-N和NH2-PSA的用量对加标回收率的影响,优化了主要的影响因素和实验条件。结果表明:5种化合物的检测在各自线性范围内线性相关性良好,相关系数r~2≥0.9954;方法回收率用三个浓度进行添加实验,回收率范围为82.5%~ 95.9%;定量限为0.5~15mug/kg。本方法前处理简单,回收率高,重现性好,可作为火锅底料中的5种罂粟壳生物碱的有效检测方法。
英文摘要A method for the determination of five poppy hull alkaloids in a pot-extinguishing saucepan was developed by dispersive solid-phase extraction coupled with pass-through solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The samples were first extracted with 80%aqueous acetonitrile.The extracts were preliminarily cleaned up by an Oasis PRiME HLB solid phase extraction column and then further purified by anhydrous sodium sulfate,octadecyl bonded silica gel adsorbent(C_(18)-N)and aminopropyl ethylenediamine adsorbent(NH2-PSA).The purified liquid was separated on a Waters CORTECS UPLCHILIC column(100mm*2.1mm,1.6um).The mobile phase was acetonitrile and 10mmol/L aqueous ammonium formate containing 0.1%(V/V)formic acid for gradient elution,and the target compounds were analyzed qualitatively and quantitatively by electrospray ionization in positive ion mode with multiple reaction ion scanning(MRM).The effects of the amounts of anhydrous sodium sulfate,C_(18)-N and NH2- PSA on the spiked recoveries were investigated.The main influencing factors and experimental conditions were optimized.The results showed that the five target compounds were linearly correlated within their corresponding linear ranges.The recoveries of the five alkaloids ranged from 82.5% to 95.9%.The limit of quantification was 0.5-15mug/kg.The established method exhibited simple pretreatment,high recoveries,good reproducibility,and can be used for the analysis of opium poppy husk alkaloids in hotpot bases.
中文关键词超高效液相色谱-串联质谱 ; 分散固相萃取 ; 火锅底料 ; 罂粟壳生物碱
英文关键词Ultra-high performance liquid chromatography-tandem mass spectrometry Dispersive solid phase extraction Hot pot soup base Alkaloids from pericarpium papaveris
类型Article
语种中文
国家中国
收录类别CSCD
WOS类目Chemistry
CSCD记录号CSCD:6953088
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/354236
作者单位吴琼, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.; 扈明洁, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.; 江海, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.; 励炯, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.; 邱红钰, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.; 李玮, 杭州市食品药品检验研究院, 杭州, 浙江 310017, 中国.
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吴琼,扈明洁,江海,等. 分散固相萃取结合通过式固相萃取净化-超高效液相色谱-串联质谱法测定火锅底料中5种罂粟壳生物碱[J],2021,37(2):1006-6144.
APA 吴琼,扈明洁,江海,励炯,邱红钰,&李玮.(2021).分散固相萃取结合通过式固相萃取净化-超高效液相色谱-串联质谱法测定火锅底料中5种罂粟壳生物碱.分析科学学报,37(2),1006-6144.
MLA 吴琼,et al."分散固相萃取结合通过式固相萃取净化-超高效液相色谱-串联质谱法测定火锅底料中5种罂粟壳生物碱".分析科学学报 37.2(2021):1006-6144.
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