天麻硫熏标志物p-hydroxybenzyl hydrogen sulfite的定量分析及稳定性研究
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摘要
特征硫熏标志物研究已成为中药质量控制的有效辅助手段。该研究建立了UPLC-MS/MS测定天麻硫熏产物p-hydroxybenzyl hydrogen sulfite的定量分析方法。应用所建立的方法对37批天麻药材进行筛查,发现27批样品是经过硫熏处理的,硫熏较严重的为云南产区的天麻样品。通过考察不同贮藏时间和加热处理下p-hydroxybenzyl hydrogen sulfite成分的稳定性,发现药材中该成分含量在8个月的贮藏期内以及正常加热处理(50,60,70,80℃)条件下是稳定可靠的。以上研究表明该硫熏产物可作为天麻硫熏标志物,具有灵敏度高、选择性好和稳定性好,为天麻质量控制和硫熏药材筛查提供参考。
Studies on the characteristic chemical markers of sulfur fumigation have become an effective auxiliary way for quality control of traditional Chinese medicine. This study established a quantitative analysis method for the determination of p-hydroxybenzyl hydrogen sulfite( p-HS) in Gastrodiae Rhizoma( GR) based on UPLC-MS/MS. Then,37 batches of GR were screened,and the results showed that 27 batches of them were sulfur-fumigated. Especially,the GR samples in Yunnan producing areas were sulfur-fumigated more seriously. Based on the stability of p-HS after different storage time and heat treatment methods,it was found that the content of p-HS was stable and reliable in the storage period of 8 months and under normal heat treatment( 50,60,70,80 ℃) conditions. In conclusion,this study shows a high sensitivity,good selectivity and good stability of p-HS,which can provide reference for the quality control and sulfur fumigation screening of GR
Studies on the characteristic chemical markers of sulfur fumigation have become an effective auxiliary way for quality control of traditional Chinese medicine. This study established a quantitative analysis method for the determination of p-hydroxybenzyl hydrogen sulfite( p-HS) in Gastrodiae Rhizoma( GR) based on UPLC-MS/MS. Then,37 batches of GR were screened,and the results showed that 27 batches of them were sulfur-fumigated. Especially,the GR samples in Yunnan producing areas were sulfur-fumigated more seriously. Based on the stability of p-HS after different storage time and heat treatment methods,it was found that the content of p-HS was stable and reliable in the storage period of 8 months and under normal heat treatment( 50,60,70,80 ℃) conditions. In conclusion,this study shows a high sensitivity,good selectivity and good stability of p-HS,which can provide reference for the quality control and sulfur fumigation screening of GR
引文
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[2]Ma X Q,Leung A K,Chan C L,et al.UHPLC UHD Q-TOF MS/MS analysis of the impact of sulfur fumigation on the chemical profile of Codonopsis Radix(Dang shen)[J].Analyst,2014,139(2):505.
[3]康传志,杨婉珍,莫歌,等.中药材二氧化硫限量标准及残留现状探讨[J].中国中药杂志,2018,43(2):242.
[4]王珊,郝丽娟,朱晶晶,等.硫磺熏蒸对杭白菊化学品质的影响[J].中国中药杂志,2014,39(8):1457.
[5]王刚,晋小军,王辉,等.硫磺熏制与贮藏期对当归二氧化硫残留量的影响[J].时珍国医国药,2014,25(2):453.
[6]中国药典.一部[S].2015:58.
[7]李超.天麻化学成分研究[D].杨凌:西北农林科技大学,2007.
[8]季德,宁子琬,张雪荣,等.不同干燥加工方法对天麻药材质量的影响[J].中国中药杂志,2016,41(14):2587.
[9]黄先敏,凌敏,杨正贤,等.不同产地天麻多糖含量测定分析[J].现代农业科技,2017(6):259.
[10]Kang C,Lai C J S,Zhao D,et al.A practical protocol for comprehensive evaluation of sulfur-fumigation of Gastrodiae Rhizoma using metabolome and health risk assessment analysis[J].J Hazard Mater,2017,340(15):221.
[11]Wu Z,Zhang J,Xu F,et al.Rapid and simple determination of polyphyllin I,II,VI,and VII in different harvest times of cultivated Paris polyphylla Smith var.yunnanensis(Franch.)Hand.-Mazz by UPLC-MS/MS and FT-IR[J].J Nat Med,2017,71(1):139.
[12]Sun C,Xu W,Zhang Y,et al.Simultaneous determination of 11compounds in Gualou Guizhi granule and pharmacokinetics study by UPLC-MS/MS[J].J Anal Method Chem,2017(2):1.
[13]康传志,吕朝耕,杨健,等.基于UPLC-MS/MS的不同主产区天麻药材质量评价研究[J].中华中医药杂志,2017,32(5):2010.
[14]康传志,蒋靖怡,杨婉珍,等.不同贮藏时间硫熏天麻化学成分及二氧化硫变化规律研究[J].中国中药杂志,2018,43(2):261.