银杏内酯C标准样品的研制

doi:10.3976/j.issn.1002-4026.2022.02.003

Abstract

Abstract:

To develop a national certified reference material (CRM) of Ginkgolide C according to the technical requirements of Directives for the work of reference materials - Reference materials - General and statistical principles for certification, Ginkgolide C was purified and obtained using silica gel column chromatography, Sephadex LH-20 gel column chromatography technology, and preparative liquid chromatography from dried leaves of Ginkgo biloba L. The structure was confirmed by UV, IR, HR-MS, ¹H-NMR, and ¹³C-NMR. The identification of thin-layer chromatography was performed, and the LC-MS technique was established. Homogeneity test, stability test, and certification analysis were conducted. Results show that the samples were stable under the storage condition of 0~4 ℃ for 2 years; the certification analysis result confirms that its purity is (99.85±0.06)%. The developed Ginkgolide C meets the technical requirements of national certified reference material per GB/T 15000.3—2008, which can be used for content determination, quality control, and detection method evaluation of Ginkgolide C and related products.

Key words: certified reference material, Ginkgolides C, purity analysis, homogeneity test, stability test, certification analysis

CLC Number:

R284.2

NING Fan-sheng,LU Yan-xiang,CAO Gui-yun,MENG Zhao-qing,Yan Hui-jiao,Wang Dai-jie. Preparation of certified reference material of Ginkgolides C[J].Shandong Science, 2022, 35(2): 18-28.

Figures/Tables 13

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References 26

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¹H	测定值(DMSO-d6,400 MHz)	文献值^[25] (DMSO-d6,400 MHz)	¹³C	测定值(DMSO-d6,100 MHz)	文献值^[25](DMSO-d6,100 MHz)
1	3.99 (1H, dd, 7.2, 3.6)	4.01 (1H, d, 7.0)	1	74.1	73.72
OH-1	4.97 (1H, d, 3.6)	4.87 (1H, brs)	2	92.3	91.90
2	4.63 (1H, d, 7.2)	4.60 (1H, d, 7.0)	3	83.3	83.01
OH-3	6.48 (1H, s)	6.39 (1H, brs)	4	98.7	98.32
6	4.97 (1H, d, 4.0)	4.98 (1H, d, 4.0)	5	66.8	66.40
7	4.06 (1H, m)	4.08 (1H, m)	6	79.5	79.11
OH-7	5.58 (1H, d, 6.2)	5.58 (1H, brs)	7	74.4	74.12
8	1.55 (1H, d, 12.4)	1.58 (1H, d, 12.5)	8	49.4	49.01
10	5.00 (1H, d, 5.6)	4.99 (1H, d, 5.0)	9	64.2	63.79
OH-10	7.54 (1H, d, 5.6)	7.43 (1H, brs)	10	69.4	69.00
12	6.10 (1H, s)	6.09 (1H, s)	11	174.3	173.94
14	2.82 (1H, q, 7.0)	2.82 (1H, q, 7.0)	12	109.9	109.57
16	1.12(3H, d, 7.0))	1.13(3H, d, 7.0)	13	171.0	170.64
t-Bu	1.09 (9H, s)	1.12 (9H, s)	14	42.0	41.56
			15	176.8	176.44
			16	8.3	7.93
			17	32.4	31.95
			18	29.4	28.92
			19	29.4	28.92
			20	29.4	28.92

瓶号	1	2	3	4	5	6	7	8	9	10
第一次抽样测量值/%	99.80	99.83	99.82	99.83	99.85	99.81	99.83	99.81	99.81	99.81
第二次抽样测量值/%	99.80	99.82	99.80	99.83	99.83	99.80	99.80	99.83	99.83	99.82
第三次抽样测量值/%	99.81	99.83	99.84	99.84	99.82	99.82	99.81	99.85	99.82	99.80
平均值/%	99.80	99.83	99.82	99.83	99.83	99.81	99.81	99.83	99.82	99.81
方差	3.3×10^-5	3.3×10^-5	4.0×10^-4	3.3×10^-5	2.3×10^-4	1.0×10^-4	2.3×10^-4	4.0×10^-4	1.0×10^-4	1.0×10^-4
总体平均值/%	99.82

变差源	方差(SS)	自由度(DF)	均方(MS)
瓶间	0.003 067	9	0.000 341
瓶内	0.003 333	20	0.000 167
总和	0.006 400	29

时间/月	测定结果/%	平均值/%	标准偏差/%	置信度为95%的扩展不确定度/%
0	99.89;99.87;99.86;99.90;99.85	99.87	0.03
6	99.82;99.82;99.83;99.81;99.80	99.82	0.02
12	99.83;99.85;99.86;99.85;99.83	99.84	0.02	0.16
18	99.83;99.82;99.85;99.84;99.82	99.83	0.02
24	99.78;99.81;99.80;99.79;99.81	99.80	0.02

序号	检测结果/%						平均值/%	标准偏差/%
序号	1-1	1-2	2-1	2-2	3-1	3-2	平均值/%	标准偏差/%
1	99.93	99.88	99.88	99.91	99.86	99.94	99.90	0.04
2	99.86	99.82	99.82	99.88	99.91	99.83	99.85	0.04
3	99.93	99.86	99.90	99.88	99.82	99.92	99.89	0.05
4	99.88	99.83	99.82	99.91	99.88	99.84	99.86	0.04
5	99.82	99.89	99.87	99.81	99.85	99.82	99.84	0.04
6	99.79	99.77	99.81	99.76	99.79	99.83	99.79	0.03
7	99.85	99.89	99.85	99.81	99.92	99.86	99.86	0.04
8	99.77	99.82	99.84	99.81	99.78	99.85	99.81	0.04

Preparation of certified reference material of Ginkgolides C

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