超高效液相-串联质谱法测定食品中罂粟壳成分

目的 建立超高效液相-串联质谱法测定食品中罂粟壳成分的分析方法。方法 罂粟壳经乙腈提取后, 经PCX固相萃取柱净化, 选择BEH HILIC柱(粒径1.7 μm, 2.1 mm×100 mm), 以含0.1%甲酸的10 mmol/L乙酸铵溶液和甲酸乙腈溶液(0.1%)作为流动相进行梯度洗脱, 在0.3 mL/min流速下, 以多反应监测(multiple reaction monitoring, MRM)扫描模式进行检测, 外标法定量。结果 吗啡、可待因在25~250 μg/kg添加浓度范围内, 回收率为68.30~80.81%。罂粟碱、那可丁、蒂巴因在0.5~2.5 μg/kg添加浓度范围内, 回收率为68.34%~78.91%。本方法罂粟碱、那可丁、蒂巴因、吗啡和可待因定量限分别为0.5、0.5、0.5、25、25 μg/kg。结论 该方法简便、快速、可靠, 可用于各种食品中罂粟壳生物碱的快速筛查与确证。     

LC-MS/MS法测定骨汤宝中3种生物碱残留量的不确定度评估

为合理表征LC-MS/MS法检测骨汤宝中罂粟碱、那可丁、蒂巴因残留量检测结果的离散性,提升检测结果的完整性和可靠性。依据DB 31/2010—2012《食品安全地方标准火锅食品中罂粟碱、吗啡、那可丁、可待因和蒂巴因的测定液相色谱-串联质谱法》对骨汤宝中的罂粟碱、那可丁和蒂巴因残留量进行测定,分析检测过程中测量不确定度的来源,进行不确定度评定,并合成总不确定度。结果表明,罂粟碱、那可丁、蒂巴因的合成相对标准不确定度分别为0.475,0.575,1.897;不确定度主要来源于标准液的配制、标准曲线的制作和试验重复性。     

盐酸罂粟碱的合成路线图解

盐酸罂粟碱是一类抗痉挛药物，在临床上应用广泛。对盐酸罂粟碱及其中间体的合成路线进行了综述，对国内两条罂粟碱合成路线进行了对比分析，并提出了具有工业化生产前景的合成路线:以邻苯二乙醚和丙烯腈为起始原料，经过加成反应、水解反应、霍夫曼酰胺降解反应，得到中间体3，4-二甲氧基苯乙胺；以邻苯二乙醚和草酰氯单乙酯为起始原料，经过傅克反应、沃尔夫-凯惜纳-黄鸣龙还原反应，得到中间体3，4-二甲氧基苯乙酸。再将上述得到的2个中间体经缩合、环合、脱氢、成盐等步骤制备盐酸罂粟碱，与其他工艺相比，该工艺原料易得，操作简单，收率高，成本低。     

HPLC测定祖卡木胶囊中罂粟碱的含量

目的建立HPLC测定祖卡木胶囊中罂粟碱含量的方法。方法色谱条件:DIKMAC8(250mm×4.6mm,5μm)色谱柱;流动相为甲醇-乙腈-1%乙酸铵-1%三乙胺(40∶20∶39∶1);流速1.0mL/min,检测波长为240nm。结果罂粟碱的线性范围为10.91～218.16ng,r=0.9999,平均回收率为97.5%,RSD=1.01%。结论本法处理简便,测定结果准确,重复性好,可用于本品的质量控制。     

LC-MS/MS法测定火锅食品中5种罂粟壳

依据JJF 1059.1—2012《测量不确定度评定与表示》和CNAS—GL06—2019《化学分析中不确定度的评估指南》中不确定度评定的基本程序,通过建立数学模型,建立了高效液相色谱串联质谱法测定火锅食品中吗啡、可待因、罂粟碱、那可丁和蒂巴因含量不确定度的分析方法。结果表明,罂粟碱、那可丁、蒂巴因、吗啡、可待因合成标准不确定度的最终结果分别为5.1×10^-2,5.0×10^-2,5.8×10^-2,8.4×10^-2,8.5×10^-2;影响测量结果不确定度的主要因素是样品回收率,样品平行试验重复性,样品提取,校准曲线拟合,标准工作溶液的配置。从校准曲线拟合这一不确定度分量可以看出,采用内标法进行测定的吗啡和可待因明显优于外标法测量的其他3种物质,可通过内标法进行测定,以降低样品基质不同所引入的不确定度。     

高效液相色谱-串联质谱法快速测定食品中5种罂粟壳生物碱

建立了高效液相色谱-串联质谱法（HPLC-MS/MS）定性定量分析食品中非法添加的吗啡、可待因、蒂巴因、罂粟碱和那可丁等5种罂粟壳生物碱。采用Capcell PAK C18 TYPE MGⅡ（5 μm×2.0 mm×150 mm）色谱柱分离,以10 mmol/L乙酸铵（pH 4.2）-乙腈为流动相,梯度洗脱,电喷雾离子源,多反应监测（MRM）模式检测。在优化的实验条件下,得到了较宽的线性范围和较低的定量检出限。吗啡和可待因的线性范围为1.0~20.0 μg/L,蒂巴因、罂粟碱和那可丁的线性范围为0.2~4.0 μg/L,相关系数均在0.999以上。食品中吗啡、可待因、蒂巴因、罂粟碱和那可丁的定量限分别为7.5、7.5、1.5、1.5、 1.5 μg/kg。方法的回收率和重现性较好,5种罂粟壳生物碱的回收率在72.2%~111.4%之间,相对标准偏差（RSD）在3.1%~8.8%之间。该方法操作简单、灵敏度高、准确可靠,可用于食品中5种非法添加罂粟壳生物碱的定量及确证分析。     

Functional Properties of Polyurethane Ureteral Stents with PLGA and Papaverine Hydrochloride Coating

Despite the obvious benefits of using ureteral stents to drain the ureters, there is also a risk of complications from 80–90%. The presence of a foreign body in the human body causes disturbances in its proper functioning. It can lead to biofilm formation on the stent surface, which may favor the development of urinary tract infections or the formation of encrustation, as well as stent fragmentation, complicating its subsequent removal. In this work, the effect of the polymeric coating containing the active substance-papaverine hydrochloride on the functional properties of ureteral stents significant for clinical practice were assessed. Methods: The most commonly clinically used polyurethane ureteral Double-J stent was selected for the study. Using the dip-coating method, the surface of the stent was coated with a poly(D,L-lactide-glycolide) (PLGA) coating containing the papaverine hydrochloride (PAP). In particular, strength properties, retention strength of the stent ends, dynamic frictional force, and the fluoroscopic visibility of the stent during X-ray imaging were determined. Results: The analysis of the test results indicates the usefulness of a biodegradable polymer coating containing the active substance for the modification of the surface of polyurethane ureteral stents. The stents coated with PLGA+PAP coating compared to polyurethane stents are characterized by more favorable strength properties, the smaller value of the dynamic frictional force, without reducing the fluoroscopic visibility.     

磁固相萃取-气相色谱-质谱法测定饮料中罂粟碱

该研究基于磁性固相萃取-气相色谱-质谱(MagneticSolidPhaseExtraction-GasChromatography-MassSpectrometry,MSPE-GC-MS)建立了饮料中罂粟碱的测定方法,成功地合成了一种具有良好吸附性能的磁性氧化石墨烯纳米复合材料,对该纳米复合材料进行了多种表征。采用单因素实验和响应面优化法(Response Surface Methodology,RSM)设计实验优化了样品吸附和解吸条件(吸附时间、吸附剂用量、溶液p H值、洗脱溶剂和解吸时间),确定最优实验条件为：磁性氧化石墨烯用量15 mg,溶液p H值7,吸附时间30 min,解吸剂(甲醇:氨水=99:1),解吸剂体积2 mL,解吸时间6 min。结果表明在优化的条件下,在0.10～2.00μg/m L的浓度范围内,所得的罂粟碱线性关系良好,其相关系数R²>0.999。利用该方法测定了3种饮料中罂粟碱的含量,在3个不同添加水平(0.10、1.00和2.00μg/m L)的加标回收率在98.43%～105.00%范围内,相对标准偏差在0.61%～3.50...     

In Vitro Effects of Papaverine on Cell Migration and Vascular Endothelial Growth Factor in Cancer Cell Lines

Papaverine (PPV) is a benzylisoquinoline alkaloid isolated from Papaver somniferum that exerts antiproliferative activity. However, several questions remain regarding the biochemical pathways affected by PPV in tumourigenic cells. In this study, the influence of PPV on cell migration (light microscopy), expression of vascular endothelial growth factor (VEGF) B, VEGF R1, VEGF R2, and phosphorylated focal adhesion kinase (pFAK) were investigated using spectrophotometry in MDA-MB-231-, A549- and DU145 cell lines. The migration assay revealed that, after 48 h, PPV (100 µM) reduced cell migration to 81%, 91%, and 71% in MDA-MB-231-, A549-, and DU145 cells, respectively. VEGF B expression was reduced to 0.79-, 0.71-, and 0.73-fold after 48 h of exposure to PPV in MDA-MB-231-, A549- and DU145 cells, while PPV exposure of 48 h increased VEGF R1 expression in MDA-MB-231- and DU145 cells to 1.38 and 1.46. A fold decrease in VEGF R1 expression was observed in A549 cells to 0.90 after exposure to 150 µM. No statistically significant effects were observed on VEGF R2- and FAK expression after exposure to PPV. This study contributes to the understanding of the effects of a phytomedicinal alkaloid compound in cancer cells and may provide novel approaches to the application of non-addictive alkaloids.     

液相色谱质谱联用法测定食品中罂粟壳成分的研究进展

食品中罂粟壳成分的检测方法尚无国家标准,液相色谱质谱联用法(liquid chromatography-tandem mass spectrometry,LC-MS-MS)具有分析范围广、分离能力强、定量定性结果可靠、检测限低、分析时间快等优点,已在食品添加剂、农药残留、兽药残留、工业染料等非法添加物的检测中得到了广泛的应用。随着研究的深入和仪器的普及,LC-MS-MS法有望成为检测食品中罂粟壳残留的标准方法。文章综述了现阶段,LC-MS-MS法检测罂粟壳成分的研究迚展,主要是仍前处理和检测条件2方面迚行分析,分别介绍了前处理的原理、方法的优化、仪器条件的选择以及近些年液质联用仪在罂粟壳成分检测方面的应用,总结了液质联用法检测罂粟壳成分可能遇到的问题及建议,为食品中罂粟壳残留监控提供参考。