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化橘红中展青霉素含量测定方法的建立
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| 篇名： | 化橘红中展青霉素含量测定方法的建立 |
| TITLE： | Establishment of the method for the content determination of patulin in Citri Grandis Exocarpium |
| 摘要： | 目的 建立一种测定化橘红药材中展青霉素含量的方法。方法采用高效液相色谱-串联三重四极杆质谱联用（HPLC-MS/MS）法。化橘红样品粉末加水溶散后经果胶酶酶解，用乙腈高速匀浆提取，提取液依次经无水硫酸镁-无水醋酸钠（4∶1，m/m）混合粉末分散固相萃取和SHIMSEN228型固相净化柱净化后，采用岛津Shim-packXR-ODS色谱柱、水-乙腈流动相、电喷雾离子源、负离子扫描、多反应监测模式测定，以基质标准曲线校正、外标法定量。结果展青霉素的检测质量浓度在5～200ng/mL范围内与峰面积成良好的线性关系（r＝0.9996）；精密度、重复性、稳定性（12h）试验的RSD均小于6%；低、中、高3种浓度加样量的平均加样回收率分别为83.90%、92.08%、92.21%（RSD分别为11.09%、5.53%、1.75%）；定量限为6μg/kg，检出限为3μg/kg。20批样品均未检出展青霉素。结论所建方法可实现对化橘红中展青霉素的快速筛查和准确定量，可为化橘红的安全性研究和质量控制提供实验依据和方法。 |
| ABSTRACT： | OBJECTIVE To establish a method for the content determination of patulin in Citri Grandis Exocarpium. METHODS High-performance liquid chromatography-triple quadrupole mass spectrometer（HPLC-MS/MS）was used for the analysis. After water-soluble dispersion and pectinase enzymolysis， the Citri Grandis Exocarpium sample was extracted by acetonitrile with high-speed homogenated. The extracted solution was conducted dispersive solid phase extraction by mixing powder of MgSO4 and NaAC （4∶1，m/m），then purified on SHIMSEN 228 solid phase purification column. Water acetonitrile was used as mobile phase， and the Shim-pack XR-ODS column was used to separate the target compound. And it was detected by electrospray ionization in the negative mode under multiple reaction monitoring， and quantified by the external standard method with matrix- matched standard correction curves. RESULTS Patulin showed good linear correlation in the concentration from 5 to 200 ng/mL （r＝0.999 6）. RSDs of precision， reproducibility and stability tests （12 h） were all lower than 6％. The average recoveries at low， medium， high concentrations were 83.9%， 92.08%， 92.21%， respectively （RSDs were 11.09%， 5.53%， 1.75%， respectively）. The limit of quantitation was 6 μg/kg and limit of detection was 3 μg/kg. Patulin was not detected in 20 batches of samples. CONCLUSIONS Established method can be used for the rapid detection and accurate quantification of patulin in Citri Grandis Exocarpium， which can provide experimental basis and method for safety study and quality control of Citri Grandis Exocarpium. |
| 期刊： | 2022年第33卷第23期 |
| 作者： | 谢思敏，陈俊妃，侯惠婵，顾利红，栗建明，王艳慧 |
| AUTHORS： | XIE Simin，CHEN Junfei，HOU Huichan，GU Lihong，LI Jianming，WANG Yanhui |
| 关键字： | 化橘红；展青霉素；高效液相色谱-串联三重四极杆质谱联用；含量测定；安全用药 |
| KEYWORDS： | Citri Grandis Exocarpium； patulin； HPLC-MS/MS； content determination； safe drug use |
| 阅读数： | 230 次 |
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