超高效液相色谱-串联质谱法快速测定镇咳祛痰药中阿片类物质的含量

建立了镇咳祛痰药中吗啡、可待因、海洛因、蒂巴因、罂粟碱、那可汀6种阿片类物质含量的LCM S/M S快速测定方法。药品经超声浸取,甲醇稀释过滤后经Waters C₁₈柱分离,以乙腈和10 mmol/L乙酸铵(含0.1%甲酸)溶液进行梯度洗脱,采用电喷雾正离子化(ESI+)、多反应监测模式进行测定。6种阿片类物质在相应的线性范围内线性均良好(r> 0.9995),检出限为吗啡0.2 ng/mL、可待因0.1 ng/mL、海洛因0.03 ng/mL、蒂巴因0.07 ng/mL、罂粟碱0.002 ng/mL、那可汀0.001 ng/mL。日内精密度为0.89%~2.5%,日间精密度为1.5%~5.5%,加标回收率在77.7%~90.5%之间。方法适用于镇咳祛痰药中吗啡、可待因、海洛因、蒂巴因、罂粟碱、那可汀6种阿片类物质的定性定量检测及质量控制。     

高效液相色谱同时测定3类食品中的5种罂粟壳生物碱

建立了同时检测3类食品中吗啡、可待因、蒂巴因、罂粟碱、那可汀5种罂粟壳生物碱含量的高效液相色谱法.试样经无水乙醇超声提取,Waters-C18(4.6 mm ×250 mm,0.5 μm)柱分离,以甲醇-0.01 mol·L-1磷酸盐为流动相梯度洗脱,通过紫外检测器进行检测.5种罂粟壳生物碱的质量浓度在10～600 m...     

气相色谱-质谱法测定火锅底料中的吗啡

正吗啡是鸦片类毒品的重要组成部分,其在罂粟壳中含量较高。罂粟壳俗称大烟壳,为罂粟科植物罂粟割取浆汁后的干燥成熟果壳,内含多种生物碱,其中含量最多的生物碱分别为吗啡、可待因、蒂巴因、罂粟碱、那可汀等~([1])。长期食用含有这类毒品的食物,会出现发冷、出虚汗、乏力、面黄肌瘦、犯困等症状,严重时可能对神经系统、消化系统造成损害,     

薄层色谱法测定罂粟籽和壳中主要生物碱的含量

据报道罂粟(Papower Somniferum L.)籽含有少量罂粟碱(Papaverine)、吗啡(Morphine)及痕量那可汀(Narcotine),罂粟壳中含有吗啡、那可汀、那萃因(Narceine)、罂粟碱、可待因(Codeine)及痕量前陶品(Protopine),这些成分均有显著的药理作用。本文用薄层色谱法测定了     

高效毛细管电泳法测定罂粟壳中生物碱的含量

采用高效毛细管电泳法测定罂粟壳中可待因、吗啡和罂粟碱的含量,结果表明可待因的加样回收率为９６．６１％,吗啡为９５．９０％,罂粟碱为９５．３７％。方法简便、准确、重现性好,可作为生物碱的质量控制方法。     

气相色谱法同时测定大麻、海洛因和鸦片中的8种组分

研究了可待因、吗啡、罂粟碱、那可汀、大麻酚、大麻二酚、四氢大麻酚和二乙酰吗啡在大口径毛细管柱上的色谱行为。采用程序升温，直接进样，在HP-1色谱柱上，使所测8种组分及内标物均获得良好的分离。据此建立了大口径毛细管气相色谱法同时对大麻、鸦片和海洛因毒品中多组分的快速测定方法。经样品测定，其平均回收率为95％-102．4％；最低检测限为0．10-0．50mg／L；相对标准偏差为0．9％-2．6％。     

固相萃取/HPLC-MS/MS检测食品中吗啡等五种罂粟壳生物碱残留

建立了同时检测食品中非法添加罂粟壳所产生的吗啡、可待因、蒂巴因、那可汀、罂粟碱残留量的固相萃取/HPLC-MS/MS方法。样品用体积分数1%三氯乙酸与乙腈混合液提取、正已烷脱脂后的净化液直接用PCX固相萃取柱净化。以乙腈-10 mmol/L乙酸铵为流动相、梯度洗脱、CR色谱柱分离、液相色谱-串联质谱联用仪检测,ESI(+)SRM模式、标准曲线外标法检测吗啡等5种生物碱。化合物标准曲线相关系数均≥0.996,定量限均为0.5,1.0,5.0μg/kg,3个浓度添加水平的回收率在62.2%~117.9%之间,相对标准偏差在5.1%~17%(n=6)之间。     

超高效液相色谱-串联质谱法快速测定火锅底料中的5种罂粟壳生物碱残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法检测火锅底料中吗啡、可待因、那可丁、罂粟碱、蒂巴因5种生物碱残留的分析方法。样品经含0.2%甲酸的乙腈提取,PRi ME HLB固相萃取小柱快速净化,ACQUITY BHE C18色谱柱(1.7μm,2.1 mm×50 mm)分离,以p H 8.0氨水溶液和乙腈作为流动相,梯度洗脱,经电喷雾正离子(ESI+)模式电离及多反应监测(MRM)测定目标化合物,采用基质标准溶液曲线法定量分析。结果表明,吗啡、可待因的线性范围为0.25~100μg/L,蒂巴因的线性范围为0.05~100μg/L,那可丁、罂粟碱的线性范围为0.05~10μg/L,相关系数均大于0.999。5种生物碱的检出限为0.9~4.5μg/kg,定量下限为3.0~15.0μg/kg;在1、5、10μg/kg(吗啡和可待因为5、25、50μg/kg)3个加标水平下的回收率为70.7%~109.6%,相对标准偏差小于11%。该方法操作快速简单、灵敏度高,适用于火锅底料中罂粟壳生物碱残留的定性与定量分析。     

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

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 C_(18)(250 mm×2.0 mm,MGⅡ 5μm)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5.0~50.0μg/L,可卡因、盐酸罂粟碱的方法线性范围为1.0~20.0μg/L,相关系数均大于0.999,方法检出限在0.1~0.8μg/kg之间,平均回收率为76.0%~111.2%,相对标准偏差RSD低于10%.     

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

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10μL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0.05～50mg....     

Separation and determination of five major opium alkaloids with mixed mode of hydrophilic/cation-exchange monolith by pressurized capillary electrochromatography

A method for the separation and determination of five major opium alkaloids (narcotine, papaverine, thebaine, codeine, and morphine) in pericarpium papaveris by pressurized CEC (pCEC) with monolithic column has been developed. Under the optimum condition, linear calibration ranges of narcotine, papaverine, thebaine, codeine, and morphine were obtained as 2-85, 2-85, 5-75, 10-65, and 10-65 microg/mL, respectively. LODs of these analytes were 1.5-6.0 microg/mL. The RSD (n=7) of the migration time and peak area were 1.94-5.24 and 4.05-8.21%, respectively. The proposed method was successfully applied to the analysis of pericarpium papaveris samples. Average recoveries of 79.0-95.9% at different fortified levels of alkaloids were achieved with RSD less than 4.6%. Meanwhile, the mechanism of the separation of the alkaloids on the monolithic column was also discussed. The result showed that the separation of alkaloids was mainly based on the mixed mode of hydrophilic interaction (HI) and cation exchange.     

TurboFlow在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法快速测定食品中违禁添加的罂粟壳

采用在线净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱(TF-UPLC-QTRAP MS)技术,建立了食品中吗啡、可待因、蒂巴因、罂粟碱、那可丁和原阿片碱6种罂粟壳标志物的快速确证检测方法。样品经0.10 mol/L盐酸提取、正己烷脱脂后,直接注入TF-UPLC-QTRAP MS进行分析。对影响净化的条件如TF-净化柱、流动相、洗脱溶液等条件进行了优化。确定以TurboFlow Cyclone MCX柱作为净化柱,Acquity BEH C_(18)柱为分析柱,甲醇-0.05%(体积分数)氨水溶液作为流动相,电喷雾正离子模式下多反应监测-触发增强子离子(MRM-IDA-EPI)扫描方式检测,以溶剂标准内标法定量。方法的检出限为0.05~0.5μg/kg,定量限为0.2~2μg/kg。平均加标回收率为81.1%~98.6%,相对标准偏差为2.9%~15.7%(n=6)。该方法灵敏、准确,适用于食品中非法添加罂粟壳的检测,已应用于实际样品的测定。     

Application of capillary zone electrophoresis in the separation and determination of the principal gum opium alkaloids

We describe the use of capillary zone electrophoresis (CZE) for the qualitative and quantitative determination of major alkaloids (i.e., thebaine, codeine, morphine, papavarine and narcotine) in gum opium involving the analysis of alkaloids without derivatization or purification. Three extractions with 2.5% w/v aqueous acetic acid quantitatively extracted major alkaloids. The separation was carried out by CZE using a 7:3 mixture of methanol and sodium acetate (100 mM, pH 3.1) at a potential of 15 kV, with UV detection at 224 nm. Spiking of pure reference alkaloid standards in the opium extract was used for peak identification. The influences of buffer composition, pH and voltage on the separation of alkaloids were studied. The detection limit of each alkaloid dissolved in methanol was found to be 850 ng/mL (morphine), 450 ng/mL (thebaine), 500 ng/mL (codeine), 550 ng/mL (papaverine), and 500 ng/mL (narcotine) at an injection pressure of 300 mbar (injection volume, 4 nL) with a signal-to-noise ratio of 3:1. The external standard method was used for the quantification of alkaloids. The calibration plot was based on linear regression analysis. The relative standard deviation (RSD) for peak area and migration time was in the range of 1.03-3.56% and 0.34-0.69%, respectively. Percentage compositions (g%) of opium alkaloids in five gum opium samples were found to be in the range of 14.45-15.95 (morphine), 2.0-3.45 (codeine), 1.32-2.73 (thebaine), 0.92-2.37 (papavarine), and 3.85-5.77 (narcotine). The method developed is suitable for the routine analysis of major gum opium alkaloids in samples of forensic importance.     

Surface-Ionization Mass Spectrometry of Opium Alkaloids

Surface ionization of the opium alkaloids morphine, codeine, thebaine, papaverine, and narcotine was investigated by mass spectrometry. It was shown that the alkaloid molecules were ionized with high efficiency through surface ionization. The mass spectra of morphine, codeine, and thebaine exhibited series of lines for quasimolecular ions with elimination of up to nine H atoms from the opiates that was accompanied by heterogeneous aromatization of the rings and their skeletal rearrangement. The results were compared with GC-MS data from electron ionization.     

高效液相色谱法检测食品中多种香料共存时的罂粟壳

 采用高效液相色谱法检测食品中多种香料共存时的罂粟壳。样品经碱化后采用氯仿 乙醇 (体积比为 9∶1)提取 ,在苯基柱上以乙腈 甲醇 水为流动相进行分离 ,外标法定量。罂粟碱 ,吗啡 ,可待因在 1 2mg/L～ 10 0mg/L范围内线性关系良好 ,平均回收率为 79.3%～ 86 .1%。该方法的专属性和准确度较高。     

Fragmentation pathways of heroin-related alkaloids revealed by ion trap and quadrupole time-of-flight tandem mass spectrometry

The electrospray ionization (ESI) ion trap and quadrupole time-of-flight (QqToF) mass spectra of heroin and seven related alkaloids, i.e., morphine, codeine, O-6-monoacetylmorphine (6-MAM), thebaine, acetylcodeine, papaverine and narcotine, have been extensively investigated in this work. The ESI mass spectrometric fragmentation pathways of protonated 6-MAM, heroin, acetylcodeine, and thebaine were comprehensively elucidated for the first time with the aid of high-resolution mass spectrometry. It was found that cleavage of the piperidine ring was the featured fragmentation route of six of the compounds, although not of papaverine and narcotine. In addition, a simple high-performance liquid chromatography (HPLC)-based separation method gave baseline resolution of all eight components. This study could play an important role in the screening for these alkaloids in different matrices by HPLC coupled to tandem mass spectrometry (MS/MS).     

罂粟碱检测方法研究进展

罂粟碱和中药罂粟壳作为临床上的常见药物及作为食品添加剂的非法使用,吸引了众多研究人员对罂粟碱检测方法的研究.本文概述了罂粟碱的结构特点和作为药物的使用情况,系统介绍了与其相关的各种检测方法,包括化学分析方法、光谱分析方法、电化学分析方法、色谱和毛细管电泳分离分析方法和免疫分析方法等,并对其检测方法的发展趋势进行了评述和展望.