热处理脱硫对硫熏党参中二氧化硫残留及含硫衍生物的影响
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摘要
目的:通过测定热处理前后硫熏党参中二氧化硫残留和含硫衍生物量的变化规律,评估硫熏党参热处理脱硫技术的可行性。方法:采用酸碱滴定法测定硫熏党参中二氧化硫残留量;采用UPLC-Q-TOF-MS/MS定性和半定量表征硫熏党参中含硫衍生物;对不同硫磺熏蒸时间和不同热处理时间的硫熏党参中二氧化硫残留量与含硫衍生物含量的变化进行相关性分析。结果:白术内酯Ⅱ含硫衍生物和白术内酯Ⅲ含硫衍生物为硫熏党参主要特征含硫衍生物。随硫熏程度的增加,党参中二氧化硫残留量显著增加,含硫衍生物的含量先增加后维持稳定,二氧化硫残留量与含硫衍生物的量之间并不一定呈正相关;随热处理程度增加,硫熏党参中二氧化硫残留量持续明显下降,但含硫衍生物的量先下降后维持稳定并保持在较高的含量水平,相关性分析结果表明热处理脱硫所致的党参药材二氧化硫残留与含硫衍生物量的变化并不一定呈正相关。结论:热处理虽然可显著降低硫熏党参中二氧化硫残留量,但药材中仍存在含量较高的含硫衍生物,不能使硫熏党参内在质量恢复到与非硫熏品质一致。因此,热处理脱硫技术不是保证硫熏党参质量的可行技术。
Objective: To evaluate the feasibility of heat-treating de-sulfur method for sulfur-fumigated Codonopsis Radix( CR) by investigating the changes in contents of sulfur dioxide residue and sulfur-containing derivatives after sulfur-fumigation. Method: Qualitative and semi-quantitative characterization of sulfur-containing derivatives was analyzed by ultra-performance liquid chromatography-quadrupole-time of flight-mass spectrometry( UPLC-Q-TOF-MS/MS),and sulfur dioxide residues were determined by acid-base titration method. Then the correlations between sulfur dioxide residues and sulfur-containing derivatives in sulfur-fumigated CR samples with different sulfur-fumigation and heat treatment extents were analyzed. Result: Atractylenolide Ⅱ and atractylenolideⅢ sulfur-containing derivatives were identified as major characteristic markers of sulfur fumigated CR. With the increase of sulfur-fumigation time,the content of sulfur dioxide residues was continuously increased,while the content of sulfur-containing derivatives was elevated at the beginning and then reached to a plateau,so there was not necessarily a positive correlation between sulfur dioxide residue and the amount of sulfur derivatives. With the increase of heat-treated time,the content of sulfur dioxide residues was continuously decreased,while the content of sulfur-containing derivatives was decreased first and remained at a high level later. There was no clear correlation between sulfur dioxide residue and sulfur-containing derivatives in different sulfur-fumigated and heat-treating desulfur degrees of CR. Conclusion: Heat-treatment could decrease the content of sulfur dioxide residue,but the content of sulfur-containing derivatives still remained at a high level,so heat treatment could not reinstate the inner quality of sulfur-fumigated CR to its non-fumigated ones. Therefore,heat-treating de-sulfur is not a feasible method for the quality assurance of sulfur-fumigated CR.
Objective: To evaluate the feasibility of heat-treating de-sulfur method for sulfur-fumigated Codonopsis Radix( CR) by investigating the changes in contents of sulfur dioxide residue and sulfur-containing derivatives after sulfur-fumigation. Method: Qualitative and semi-quantitative characterization of sulfur-containing derivatives was analyzed by ultra-performance liquid chromatography-quadrupole-time of flight-mass spectrometry( UPLC-Q-TOF-MS/MS),and sulfur dioxide residues were determined by acid-base titration method. Then the correlations between sulfur dioxide residues and sulfur-containing derivatives in sulfur-fumigated CR samples with different sulfur-fumigation and heat treatment extents were analyzed. Result: Atractylenolide Ⅱ and atractylenolideⅢ sulfur-containing derivatives were identified as major characteristic markers of sulfur fumigated CR. With the increase of sulfur-fumigation time,the content of sulfur dioxide residues was continuously increased,while the content of sulfur-containing derivatives was elevated at the beginning and then reached to a plateau,so there was not necessarily a positive correlation between sulfur dioxide residue and the amount of sulfur derivatives. With the increase of heat-treated time,the content of sulfur dioxide residues was continuously decreased,while the content of sulfur-containing derivatives was decreased first and remained at a high level later. There was no clear correlation between sulfur dioxide residue and sulfur-containing derivatives in different sulfur-fumigated and heat-treating desulfur degrees of CR. Conclusion: Heat-treatment could decrease the content of sulfur dioxide residue,but the content of sulfur-containing derivatives still remained at a high level,so heat treatment could not reinstate the inner quality of sulfur-fumigated CR to its non-fumigated ones. Therefore,heat-treating de-sulfur is not a feasible method for the quality assurance of sulfur-fumigated CR.
引文
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[2]刘静静,刘晓,李松林,等.硫磺熏蒸中药材及饮片的研究现状[J].中草药,2010,41(8):1403-1406.
[3]赵玉英,张娟娟,王颖莉.硫磺熏蒸前后党参红外光谱特征变化规律[J].中国实验方剂学杂志,2015,21(10):63-66.
[4]孟召全.硫熏法对党参有效成分含量的影响[J].中国中医药信息杂志,2010,17(S1):37-38.
[5]李成义,魏学明,王明伟,等.硫熏对党参中党参炔苷含量的影响[J].中国现代中药,2010,12(12):11-13.
[6]杨军宣,郭振宇,张毅,等.不同党参饮片贮藏期有效成分的稳定性研究[J].中药材,2018,41(1):89-92.
[7] MA X Q,Leung A K,CHAN C L,et al. UHPLC UHD QTOF MS/MS analysis of the impact of sulfur fumigation on the chemical profile of Codonopsis Radix(Dangshen)[J]. Analyst(Lond),2014,139(2):505-516.
[8]刘成松,王玉萍,史彦斌,等.硫磺熏蒸党参对小鼠免疫功能的影响[J].中药材,2014,37(11):1969-1972.
[9]李萍,彭百承,甄丹丹,等. 3种含硫量不同的党参药效比较[J].中国实验方剂学杂志,2010,16(11):175-176,179.
[10]国家药典委员会.中华人民共和国药典.一部[M].北京:中国医药科技出版社,2015:281-282.
[11]国家药典委员会.中华人民共和国药典.四部[M].北京:中国医药科技出版社,2015:208.
[12] SUN X,CUI X B,WEN H M,et al. Influence of sulfur fumigation on the chemical profiles of Atractylodes macrocephala Koidz. evaluated by UFLC-QTOF-MS combined with multivariate statistical analysis[J]. J Pharmaceut Biomed,2017,141:19-31.
[13] MA B,KAN W L,ZHU H,et al. Sulfur fumigation reducing systemic exposure of ginsenosides and weakening immunomodulatory activity of ginseng[J]. J Ethnopharmacol,2017,195:222-230.
[14] KONG M,LIU H H,WU J,et al. Effects of sulfurfumigation on the pharmacokinetics,metabolites and analgesic activity of Radix Paeoniae Alba[J]. J Ethnopharmacol,2017,212:95-105.
[15]陆兔林,宁子琬,单鑫,等.硫磺熏蒸对中药材化学成分和药理作用影响的研究进展[J].中国中药杂志,2014,39(15):2796-2800.
[16]丁喜炎,季琳,程雪,等.不同硫熏替代技术的黄芪药材对小鼠免疫功能影响研究[J].中国中药杂志,2016,41(15):2819-2823.