通腑泻下颗粒指纹图谱的建立及7种成分的定量分析

doi:10.19894/j.issn.1000-0518.230249

摘要/Abstract

摘要：

建立通腑泻下颗粒（TongFu XieXia Granules， TFXXG）的高效液相色谱（HPLC）指纹图谱，并同时测定大黄素、大黄酚、大黄酸、芦荟大黄素、大黄素甲醚、厚朴酚以及和厚朴酚的含量。采用Waters Symmetry C₁₈（2.1 mm×150 mm，3.5 μm）色谱柱，以0.1%磷酸水溶液（A）和甲醇（B）为流动相梯度洗脱；流速为0.4 mL/min；柱温为30 ℃；检测波长为254 nm；进样量为10 μL。建立10批TFXXG的指纹图谱，并采用“中药色谱指纹图谱相似度评价系统”（2012版）计算相似度；测定大黄素、大黄酚、大黄酸、芦荟大黄素、大黄素甲醚、厚朴酚以及和厚朴酚的含量。结果表明，10批TFXXG共确定出25个共有峰，相似度均在0.950以上；共指认出12个共有峰，分别为芥子碱硫氰酸盐、咖啡酸、松果菊苷、柚皮苷、新橙皮苷、芦荟大黄素、大黄酸、厚朴酚、和厚朴酚、大黄酚、大黄素以及大黄素甲醚。其中，芦荟大黄素、大黄酸、厚朴酚、和厚朴酚、大黄素、大黄酚以及大黄素甲醚的含量分别为0.1244~0.1304、0.4271~0.4387、3.0479~3.0853、1.2910~1.3039、0.2427~0.2523、0.7718~0.7897和0.5085~0.5249 mg/g。本文所建指纹图谱和定量分析方法重复性好，可操作性强，可用于控制TFXXG的质量。

关键词: 通腑泻下颗粒, 高效液相色谱法, 指纹图谱, 含量测定

Abstract:

The high performance liquid chromatographic （HPLC） fingerprints of TongFu XieXia Granules （TFXXG） are established， and the contents of Emodin， Chrysophanic acid， Rhein， Aloeemodin， Physcion， Magnolol and Honokiol are simultaneously determined. The separation is performed on a Waters Symmetry C18 column （2.1 mm × 150 mm， 3.5 μm） with a gradient elution of 0.1% aqueous phosphoric acid （A） and methanol （B） as the mobile phases， at a flow rate of 0.4 mL/min， with the column temperature at 30 ℃， the detection wavelength at 254 nm， and the injection volume of 10 μL. The fingerprints of 10 batches of TFXXG are established， and the similarity is calculated by using the “Evaluation system for similarity of chromatographic fingerprints of traditional Chinese medicines” （2012 version）； the contents of Emodin， Chrysophanic acid， Rhein， Aloeemodin， Physcion， Magnolol and Honokiol are determined. The results show that a total of 25 common peaks is identified in the 10 batches of TFXXG， and the similarities are all above 0.950； a total of 12 common peaks are identified， which are Sinapine thiocyanate， Caffeic acid， Echinacoside， Naringin， Neohesperidin， Aloeemodin， Rhein， Magnolol， Honokiol， Emodin， Chrysophanic acid and Physcion， respectively. The contents of Aloeemodin， Rhein， Magnolol， Honokiol， Emodin， Chrysophanic acid and Physcion are 0.1244~0.1304， 0.4271~0.4387， 3.0479~3.0853， 1.2910~1.3039， 0.2427~0.2523， 0.7718~0.7897 and 0.5085~0.5249 mg/g， respectively. The fingerprints and quantitative analytical methods constructed in this paper are reproducible and operable， and can be used to control the quality of TFXXG.

Key words: TongFu XieXia Granules, High performance liquid chromatographic, Fingerprints, Content determination

中图分类号:

O656.3

朴禹涵, 马丽婷, 罗静, 刘书晗, 白若冰, 张若妍, 越皓, 郑飞. 通腑泻下颗粒指纹图谱的建立及7种成分的定量分析[J]. 应用化学, 2024, 41(4): 577-585.

Yu-Han PIAO, Li-Ting MA, Jing LUO, Shu-Han LIU, Ruo-Bing BAI, Ruo-Yan ZHANG, Hao YUE, Fei ZHENG. Fingerprints and Determination of Seven Components of TongFu XieXia Granules[J]. Chinese Journal of Applied Chemistry, 2024, 41(4): 577-585.

图/表 7

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Compounds	Regression equation	R²	Linear range/（mg·mL^-1）
Aloeemodin	y=10.934x－6.1889	0.999 2	0.002~0.02
Rhein	y=0.5493x+2.4871	0.999 0	0.004~0.04
Magnolol	y=0.452x+3.0233	0.999 0	0.006~0.06
Honokiol	y=0.5751x+2.5367	0.999 0	0.008~0.08
Chrysophanic acid	y=0.3999x－0.6025	0.999 0	0.005~0.05
Emodin	y=1.0526x－1.5943	0.999 5	0.030~0.30
Physcion	y=1.5132x+0.3476	0.999 2	0.014~0.14

Compounds	Regression equation	R²	Linear range/（mg·mL^-1）
Aloeemodin	y=10.934x－6.1889	0.999 2	0.002~0.02
Rhein	y=0.5493x+2.4871	0.999 0	0.004~0.04
Magnolol	y=0.452x+3.0233	0.999 0	0.006~0.06
Honokiol	y=0.5751x+2.5367	0.999 0	0.008~0.08
Chrysophanic acid	y=0.3999x－0.6025	0.999 0	0.005~0.05
Emodin	y=1.0526x－1.5943	0.999 5	0.030~0.30
Physcion	y=1.5132x+0.3476	0.999 2	0.014~0.14

Compounds	Weighingquantity/g	Originalquantity/μg	Addition/μg	Measured quantity/μg	Recoveryrate/%	Average recovery rate/%	RSD/%（n=6）
Aloeemodin	0.040 1	5.1	5.1	10.1	98.92	100.63	1.09
	0.040 1	5.1	5.1	10.2	99.91
	0.040 3	5.1	5.1	10.2	101.61
	0.040 2	5.1	5.1	10.2	100.39
	0.040 4	5.1	5.1	10.2	101.58
	0.040 2	5.1	5.1	10.3	101.39
Rhein	0.040 1	17.3	17.3	34.5	99.61	99.60	1.16
	0.040 1	17.3	17.3	34.3	98.40
	0.040 3	17.2	17.3	34.4	99.42
	0.040 2	17.2	17.3	34.4	99.00
	0.040 4	17.2	17.3	34.8	101.81
	0.040 2	17.2	17.3	34.4	99.35
Magnolol	0.040 1	122.4	122.7	244.7	99.69	100.10	0.94
	0.040 1	122.4	122.7	247.5	101.94
	0.040 3	122.8	122.7	245.3	99.81
	0.040 2	123.2	122.7	246.0	100.12
	0.040 4	122.7	122.7	245.0	99.72
	0.040 2	123.2	122.7	245.0	99.32
Honokiol	0.040 1	51.8	51.9	103.5	99.69	100.16	0.70
	0.040 1	51.8	51.9	103.4	99.37
	0.040 3	51.5	51.9	103.9	100.86
	0.040 2	51.7	51.9	104.1	101.02
	0.040 4	51.5	51.9	103.6	100.43
	0.040 2	51.7	51.9	103.4	99.60
Emodin	0.040 1	9.9	9.9	19.9	101.44	100.72	1.06
	0.040 1	9.9	9.9	19.7	99.93
	0.040 3	9.8	9.9	19.9	101.50
	0.040 2	9.8	9.9	19.9	101.43
	0.040 4	9.8	9.9	19.8	101.08
	0.040 2	9.8	9.9	19.6	98.91
Chrysophanic acid	0.040 1	31.4	31.4	63.2	101.33	101.01	0.60
	0.040 1	31.4	31.4	62.8	100.10
	0.040 3	31.2	31.4	62.8	100.54
	0.040 2	31.3	31.4	63.1	101.09
	0.040 4	31.2	31.4	63.1	101.77
	0.040 2	31.3	31.4	63.1	101.22
Physcion	0.040 1	20.5	20.5	41.0	99.88	100.64	0.58
	0.040 1	20.5	20.5	41.1	100.64
	0.040 3	20.4	20.5	41.1	100.86
	0.040 2	20.4	20.5	41.0	100.37
	0.040 4	20.4	20.5	41.0	100.49
	0.040 2	20.4	20.5	41.3	101.61

Compounds	Weighingquantity/g	Originalquantity/μg	Addition/μg	Measured quantity/μg	Recoveryrate/%	Average recovery rate/%	RSD/%（n=6）
Aloeemodin	0.040 1	5.1	5.1	10.1	98.92	100.63	1.09
	0.040 1	5.1	5.1	10.2	99.91
	0.040 3	5.1	5.1	10.2	101.61
	0.040 2	5.1	5.1	10.2	100.39
	0.040 4	5.1	5.1	10.2	101.58
	0.040 2	5.1	5.1	10.3	101.39
Rhein	0.040 1	17.3	17.3	34.5	99.61	99.60	1.16
	0.040 1	17.3	17.3	34.3	98.40
	0.040 3	17.2	17.3	34.4	99.42
	0.040 2	17.2	17.3	34.4	99.00
	0.040 4	17.2	17.3	34.8	101.81
	0.040 2	17.2	17.3	34.4	99.35
Magnolol	0.040 1	122.4	122.7	244.7	99.69	100.10	0.94
	0.040 1	122.4	122.7	247.5	101.94
	0.040 3	122.8	122.7	245.3	99.81
	0.040 2	123.2	122.7	246.0	100.12
	0.040 4	122.7	122.7	245.0	99.72
	0.040 2	123.2	122.7	245.0	99.32
Honokiol	0.040 1	51.8	51.9	103.5	99.69	100.16	0.70
	0.040 1	51.8	51.9	103.4	99.37
	0.040 3	51.5	51.9	103.9	100.86
	0.040 2	51.7	51.9	104.1	101.02
	0.040 4	51.5	51.9	103.6	100.43
	0.040 2	51.7	51.9	103.4	99.60
Emodin	0.040 1	9.9	9.9	19.9	101.44	100.72	1.06
	0.040 1	9.9	9.9	19.7	99.93
	0.040 3	9.8	9.9	19.9	101.50
	0.040 2	9.8	9.9	19.9	101.43
	0.040 4	9.8	9.9	19.8	101.08
	0.040 2	9.8	9.9	19.6	98.91
Chrysophanic acid	0.040 1	31.4	31.4	63.2	101.33	101.01	0.60
	0.040 1	31.4	31.4	62.8	100.10
	0.040 3	31.2	31.4	62.8	100.54
	0.040 2	31.3	31.4	63.1	101.09
	0.040 4	31.2	31.4	63.1	101.77
	0.040 2	31.3	31.4	63.1	101.22
Physcion	0.040 1	20.5	20.5	41.0	99.88	100.64	0.58
	0.040 1	20.5	20.5	41.1	100.64
	0.040 3	20.4	20.5	41.1	100.86
	0.040 2	20.4	20.5	41.0	100.37
	0.040 4	20.4	20.5	41.0	100.49
	0.040 2	20.4	20.5	41.3	101.61

Compounds	S1	S2	S3	S4	S5	S6	S7	S8	S9	S10
Aloeemodin	0.125 8	0.124 4	0.127 1	0.129 4	0.128 0	0.124 4	0.126 9	0.129 4	0.130 4	0.127 6
Rhein	0.433 9	0.433 0	0.436 9	0.432 5	0.427 1	0.429 3	0.431 9	0.432 8	0.438 7	0.437 2
Magnolol	3.081 0	3.059 5	3.047 9	3.074 6	3.085 3	3.071 5	3.065 9	3.068 6	3.067 0	3.068 1
Honokiol	1.303 9	1.298 6	1.297 9	1.291 0	1.295 5	1.298 8	1.294 5	1.298 9	1.300 6	1.299 9
Emodin	0.244 8	0.242 7	0.246 4	0.245 4	0.245 9	0.252 3	0.246 3	0.244 4	0.250 6	0.251 2
Chrysophanic acid	0.786 0	0.784 8	0.789 7	0.780 5	0.791 9	0.771 8	0.781 4	0.789 4	0.782 4	0.784 8
Physcion	0.523 7	0.524 9	0.521 9	0.515 1	0.520 9	0.515 2	0.524 1	0.517 2	0.508 5	0.519 1