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1.江西中医药大学 药学院,南昌 330004
2.建昌帮药业有限公司,江西 抚州 344700
张涛,硕士,从事中药炮制研究,E-mail:1512337515@qq.com
姚方程,工程师,从事中药生产及炮制技术研究工作,Tel:0794-7222866,E-mail:398639920@qq.com
张金莲,博士,教授,从事中药学及中药炮制学的教学及科学研究,Tel:0791-87118995,E-mail:jxjzzjl@163.com; *
收稿日期:2021-06-24,
网络出版日期:2021-08-17,
纸质出版日期:2022-07-20
移动端阅览
张涛,邓亚羚,陈西勇等.基于HS-GC-MS考察建昌帮炆法对何首乌气味形成的影响[J].中国实验方剂学杂志,2022,28(14):134-141.
ZHANG Tao,DENG Yaling,CHEN Xiyong,et al.Effect of Jianchangbang Braising Method on Formation of Odor of Polygoni Multiflori Radix Based on HS-GC-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(14):134-141.
张涛,邓亚羚,陈西勇等.基于HS-GC-MS考察建昌帮炆法对何首乌气味形成的影响[J].中国实验方剂学杂志,2022,28(14):134-141. DOI: 10.13422/j.cnki.syfjx.20211857.
ZHANG Tao,DENG Yaling,CHEN Xiyong,et al.Effect of Jianchangbang Braising Method on Formation of Odor of Polygoni Multiflori Radix Based on HS-GC-MS[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(14):134-141. DOI: 10.13422/j.cnki.syfjx.20211857.
目的
2
通过比较不同产地何首乌经江西建昌帮炆法和2020年版《中华人民共和国药典》收载的蒸法炮制前后饮片挥发性成分的差异,考察炮制方法对何首乌气味形成的影响。
方法
2
采用顶空气相色谱-质谱法(HS-GC-MS)检测3个产地不同炮制方法共30批何首乌样品的挥发性成分,气相色谱条件为程序升温(起始温度40 ℃,以5 ℃·min
-1
升至150 ℃,再以10 ℃·min
-1
升至195 ℃),载气高纯度氦气,分流比10∶1;质谱条件为电子轰击离子源(EI),检测范围
m
/
z
50~650,利用峰面积归一化法计算各组分的相对质量分数;运用精密色差仪测定不同炮制品的色度值,采用OriginPro 2021探讨色度值与挥发性成分相对含量的相关性;运用SIMCA 14.1对各样品数据进行主成分分析(PCA)和正交偏最小二乘法-判别分析(OPLS-DA),根据变量重要性投影(VIP)值
>
1.5的原则筛选得到不同炮制品之间的差异性成分,探究何首乌及其炮制品不同气味形成的物质基础。
结果
2
共鉴定出59种挥发性成分,其中何首乌34种、炆何首乌33种、制何首乌27种;参数红绿色值(
a
*
)、黄蓝色值(
b
*
)、总色度值(
E
*
ab
)与各挥发性成分相对含量均无显著相关性;而明度值(
L
*
)与2-甲基-2-丁烯醛、2-甲基四氢呋喃-3-酮和2,3-二氢-3,5-二羟基-6-甲基-4(H)-吡喃-4-酮的相对含量存在明显负相关(
P
<
0.05)。PCA及OPLS-DA结果表明,何首乌及其不同炮制品之间存在明显差异,但同一炮制方法不同产地的样品之间差异不明显。己酸、壬酸、合成樟脑等刺激性臭味成分在炮制后含量降低;而2-甲基-2-丁烯醛、糠醛、5-羟甲基糠醛、甲基麦芽酚、糠醇等成分具有甜香味,在炮制后含量升高。糠醛、5-甲基-2-呋喃甲醇、5-羟甲基糠醛等香味成分的含量在炆何首乌中显著高于制何首乌。
结论
2
不同炮制方法对何首乌气味的影响大于产地;颜色参数
L
*
与挥发性成分相对含量存在显著相关性;何首乌的“生”味可能与己酸、壬酸、合成樟脑等挥发性成分有关,炮制后的“香味”与2-甲基-2-丁烯醛、糠醛、5-羟甲基糠醛、甲基麦芽酚、糠醇等的含量升高有关。
Objective
2
By comparing the difference of volatile components of the decoction pieces before and after being processed by braising method of Jianchangbang and steaming method included in the 2020 edition of
Chinese Pharmacopoeia
, the influence of processing methods on the flavor formation of Polygoni Multiflori Radix
(PMR) was compared.
Method
2
Headspace-gas chromatography-mass spectrometry (HS-GC-MS) was used to detect the volatile components of 30 batches of PMR samples from 3 origins with 3 processing methods. The GC was performed under programmed temperature (starting temperature of 40 ℃, rising to 150 ℃ at 5 ℃·min
-1
, and then rising to 195 ℃ at 10 ℃·min
-1
) with high purity helium as carrier gas and the split ratio of 10∶1. Mass spectrometry conditions were electron impact ion source (EI) and the detection range of
m
/
z
50-650, the peak area normalization method was used to calculate the relative mass fraction of each component. The chromaticity values of different processed products were measured by a precision colorimeter, the relationship between chromaticity values and relative contents of volatile components was investigated by OriginPro 2021, principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed on the sample data by SIMCA14.1. The differential components of different processed products of PMR were screened according to the principle of variable importance in the projection (VIP) value
>
1.5, and the material basis of different odor formation of PMR and its processed products was explored.
Result
2
A total of 59 volatile components were identified, among which 34 were raw products, 33 were braised products, and 27 were steamed products. PCA and OPLS-DA results showed that there were significant differences between the three, but there was no significant difference between samples from different origins of the same processing method. Color parameters of
a
*
,
b
*
,
E
*
ab
had no significant correlation with contents of volatile components, while
L
*
was negatively correlated with contents of 2-methyl-2-butenal, 2-methyltetrahydrofuran-3-one and 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one (
P
<
0.05). The contents of pungent odor components such as caproic acid, nonanoic acid and synthetic camphor decreased after processing, while the contents of sweet flavor components such as 2-methyl-2-butenal, furfural and 5-hydroxymethylfurfural increased after processing, and the contents of furfural, 5-methyl-2-furanmethanol, 5-hydroxymethylfurfural and other aroma components in the braised products were significantly higher than that in the steamed products.
Conclusion
2
HS-GC-MS can quickly identify the volatile substance basis that causes the different odors of PMR and its processed products. The effect of processing methods on the odor is greater than that of origin. There is a significant correlation between the color parameter of
L
*
and contents of volatile components, the "raw" taste of PMR may be related to volatile components such as caproic acid, pelargonic acid and synthetic camphor, the "flavor" after processing may be related to the increase of the contents of 2-methyl-2-butenal, furfural, 5-hydroxymethylfurfural, methyl maltol and furfuryl alcohol.
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