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目的:将功能化磁性纳米颗粒2-氨基-5-巯基-1,3,4-噻二唑—(3-巯基丙基)三甲氧基硅烷—磁性纳米颗粒用于生脉饮(党参方)中黄曲霉毒素B1的净化富集处理,建立基于功能化磁性纳米颗粒的磁性固相萃取-高效液相色谱-荧光法,测定生脉饮(党参方)中黄曲霉毒素B1含量。方法:制备功能化磁性纳米颗粒,建立磁性固相萃取-高效液相色谱-荧光法对生脉饮(党参方)中黄曲霉毒素B1的含量进行测定。萃取条件:磁性纳米颗粒用量150 mg,吸附搅拌时间10 min,洗脱剂二氯甲烷-丙酮(2∶1),洗脱剂用量9 m L,解吸附搅拌时间8 min。色谱条件:采用C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-甲醇-0.1%甲酸水(20∶20∶60),等度洗脱;流速1.0 mL·min~(-1);柱温25℃;荧光检测器检测,激发波长360 nm,发射波长440 nm。结果:获得了优化的磁性固相萃取条件,对建立起的方法进行方法学考察,结果表明黄曲霉毒素B1浓度在0.3~10 ng·mL~(-1)范围内线性关系良好(r大于0.999 5);加样回收率为93.8%~103.5%,检测限为0.07 ng·mL~(-1),定量限为0.21 ng·mL~(-1);所测9批样品黄曲霉毒素B1含量为1.04~1.93 ng·mL~(-1)。结论:成功建立了基于功能化磁性纳米颗粒的磁性固相萃取-高效液相色谱-荧光法,并将该法用于生脉饮(党参方)中黄曲霉毒素B1的含量测定。本研究为建立一种低成本检测中成药中黄曲霉毒素的方法提供了依据,为更好地保障中药安全使用提供了技术支持。
OBJECTIVE: To use functional magnetic nanoparticle 2-amino-5-mercapto-1,3,4-thiadiazole- (3-mercaptopropyl) trimethoxysilane magnetic nanoparticles for Sheng Mai Yin (Dangshen Fang) Aflatoxin B1 purification and enrichment, magnetic solid-phase extraction-high performance liquid chromatography-fluorescence method based on functionalized magnetic nanoparticles was established to determine the content of aflatoxin B1 in Shengmai Yin (Dangshenfang). Methods: Functional magnetic nanoparticles were prepared and the content of aflatoxin B1 in Shengmai Yin (Dangshenfang) was determined by magnetic solid phase extraction - high performance liquid chromatography - fluorescence method. Extraction conditions: the amount of magnetic nanoparticles 150 mg, adsorption stirring time 10 min, eluent dichloromethane - acetone (2: 1), the amount of eluent 9 m L, desorption and stirring time 8 min. Chromatographic conditions: acetonitrile-methanol-0.1% formic acid water (20:20:60) was used as mobile phase on C18 column (4.6 mm × 250 mm, 5 μm) with isocratic elution; flow rate was 1.0 mL · min -1 ); Column temperature 25 ℃; fluorescence detector detection, excitation wavelength 360 nm, emission wavelength 440 nm. Results: The optimized conditions of magnetic solid-phase extraction were obtained. The methodology was investigated. The results showed that the linearity of aflatoxin B1 ranged from 0.3 to 10 ng · mL ~ (-1) (r> 0.999 5) .The recoveries were 93.8% -103.5%, the detection limit was 0.07 ng · mL -1, and the limit of quantification was 0.21 ng · mL -1. The contents of aflatoxin B1 1.04 ~ 1.93 ng · mL ~ (-1). CONCLUSION: Magnetic solid-phase extraction-high performance liquid chromatography-fluorescence method based on functionalized magnetic nanoparticles was successfully established. The method was applied to the determination of aflatoxin B1 in Shengmai Yin (Dangshenfang). This study provides a basis for the establishment of a low-cost method for the determination of aflatoxins in proprietary Chinese medicines and provides technical support for better safe use of traditional Chinese medicines.