目的:测定马蓝中水分、总灰分、酸不溶性灰分、浸出物的含量,为马蓝药材质量标准的建立提供参考依据。方法:依据《中国药典》2020年版四部通则下方法,分别对24个不同批次的马蓝药材中水分、总灰分、酸不溶灰分和浸出物进行测定。结果:24个批次的马蓝水分含量范围在7.68%~9.37%,总灰分含量范围在7.32%~9.94%,酸不溶性灰分范围在0.51%~1.01%,浸出物范围在14.46%~26.76%。结论:建议马蓝药材的水分暂定不超过12%,总灰分不超过10%,酸不溶性灰分不超过3%,浸出物不少于10%。 Objective: To determine the contents of moisture, ash and extract in S. cusia, and to provide reference for the establishment of quality standard of S. cusia. Methods: The moisture, total ash, acid-insoluble ash and extract of 24 different batches of S. cusia were determined according to the method in the general principles of the 2020 edition of Chinese Pharmacopoeia. Results: The moisture content of 24 batches of S. cusia ranged from 7.68 % to 9.37 %, the total ash content ranged from 7.32 % to 9.94 %, the acid insoluble ash content ranged from 0.51 % to 1.01 %, and the extract ranged from 14.46 % to 26.76 %. Conclusion: It is recommended that the moisture content of the medicinal material should not exceed 12 %, the total ash content should not exceed 10 %, the acid insoluble ash content should not exceed 3 %, and the extract should not be less than 10 %.
目的:测定马蓝中水分、总灰分、酸不溶性灰分、浸出物的含量,为马蓝药材质量标准的建立提供参考依据。方法:依据《中国药典》2020年版四部通则下方法,分别对24个不同批次的马蓝药材中水分、总灰分、酸不溶灰分和浸出物进行测定。结果:24个批次的马蓝水分含量范围在7.68%~9.37%,总灰分含量范围在7.32%~9.94%,酸不溶性灰分范围在0.51%~1.01%,浸出物范围在14.46%~26.76%。结论:建议马蓝药材的水分暂定不超过12%,总灰分不超过10%,酸不溶性灰分不超过3%,浸出物不少于10%。
马蓝,水分,灰分,浸出物,质量标准
Wuhai Yang1, Zihan Huang1, Hao Yu2, Ye Yang1, Zhikun Wu1*
1College of Pharmacy, Guizhou University of Traditional Chinese Medicine, Guiyang Guizhou
2Guizhou Qingyulan Agricultural Investment Co., Ltd., Rongjiang, Guizhou
Received: Apr. 25th, 2024; accepted: May 23rd, 2024; published: May 30th, 2024
Objective: To determine the contents of moisture, ash and extract in S. cusia, and to provide reference for the establishment of quality standard of S. cusia. Methods: The moisture, total ash, acid-insoluble ash and extract of 24 different batches of S. cusia were determined according to the method in the general principles of the 2020 edition of Chinese Pharmacopoeia. Results: The moisture content of 24 batches of S. cusia ranged from 7.68 % to 9.37 %, the total ash content ranged from 7.32 % to 9.94 %, the acid insoluble ash content ranged from 0.51 % to 1.01 %, and the extract ranged from 14.46 % to 26.76 %. Conclusion: It is recommended that the moisture content of the medicinal material should not exceed 12 %, the total ash content should not exceed 10 %, the acid insoluble ash content should not exceed 3 %, and the extract should not be less than 10 %.
Keywords:Strobilanthes cusia, Moisture, Ash, Extract, Quality Standard
Copyright © 2024 by author(s) and beplay安卓登录
This work is licensed under the Creative Commons Attribution International License (CC BY 4.0).
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马蓝Baphicacanthus cusia (Nees) Bremek.为爵床科(Acanthaceae)马蓝属植物,广泛分布于我国西南、华南和华东等地区且在中部、南部和西南部都有栽培利用 [
国内马蓝药材的产地与种质资源较为复杂,市面上伪品假货猖獗,其与正品品质相比差距甚大,对药厂原料甚至临床疗效产生了极大的影响。市面上马蓝药材质量参差不齐,存在着严重的质量问题。为此,本文参照2020版《中国药典》方法( [
实验所用仪器见表1。
仪器名称 | 型号 | 厂家名称 |
---|---|---|
四孔电热恒温水浴锅 | HH-4 | 常州市普达教学仪器有限公司 |
电热恒温鼓风干燥箱 | GZX-GF101-2-S-II | 上海贺德实验设备有限公司 |
箱式电阻炉 | 4-10 | 北京市永光明医疗仪器厂 |
KSW电炉温度控制器 | 2001 | 北京市永光明医疗仪器厂 |
万分之一分析天平 | BSA224S | 赛多利斯科学仪器北京有限公司 |
表1. 实验仪器
实验所用化学试剂见表2。
试剂名称 | 批次 | 级别 | 厂家名称 |
---|---|---|---|
乙醇 | 20180915 | 分析纯 | 天津市富宇精细化工有限公司 |
盐酸 | 20150201 | 分析纯 | 重庆川化工集团有限公司 |
表2. 实验试剂
马蓝样品均采自贵州省榕江县,具体信息见表3。
编号 | 经度 | 纬度 | 海拔(m) |
---|---|---|---|
S1 | 108.348098˚E | 26.155978˚N | 510 |
S2 | 108.645080˚E | 26.029952˚N | 726 |
S3 | 108.270882˚E | 25.852825˚N | 303 |
S4 | 108.417285˚E | 26.064110˚N | 744 |
S5 | 108.429728˚E | 26.117189˚N | 834 |
S6 | 108.291471˚E | 26.163096˚N | 801 |
S7 | 108.526590˚E | 25.836308˚N | 581 |
S8 | 108.355588˚E | 26.262133˚N | 998 |
S9 | 108.629808˚E | 26.421306˚N | 885 |
S10 | 108.432066˚E | 26.192606˚N | 788 |
S11 | 108.359223˚E | 26.047757˚N | 585 |
S12 | 108.197599˚E | 25.714552˚N | 622 |
S13 | 108.498739˚E | 26.145169˚N | 859 |
S14 | 108.398330˚E | 26.152490˚N | 712 |
S15 | 108.324600˚E | 26.199123˚N | 620 |
S16 | 108.334460˚E | 26.241927˚N | 633 |
S17 | 108.556472˚E | 26.165657˚N | 380 |
S18 | 108.329106˚E | 26.181243˚N | 524 |
S19 | 108.516144˚E | 26.240242˚N | 635 |
S20 | 108.376324˚E | 26.003016˚N | 335 |
S21 | 108.334909˚E | 26.310331˚N | 796 |
S22 | 108.459288˚E | 25.913349˚N | 370 |
S23 | 108.398330˚E | 26.152490˚N | 712 |
S24 | 108.622593˚E | 26.018720˚N | 458 |
表3. 马蓝样品信息
按照2020年版《中国药典》第四部0832水分测定法项目下的第二法(烘干法)进行测定 [
批次 | 取样量(g) | 水分(%) | 平均值(%) | RSD (%) |
---|---|---|---|---|
S1 | 2.0000 | 8.02 | 8.07 | 0.57 |
2.0000 | 8.11 | |||
2.0001 | 8.08 | |||
S2 | 2.0000 | 8.14 | 8.07 | 0.81 |
2.0001 | 8.41 | |||
2.0001 | 8.53 | |||
S3 | 1.9999 | 7.97 | 7.99 | 0.43 |
2.0000 | 8.01 | |||
2.0002 | 8.07 | |||
S4 | 2.0001 | 8.39 | 8.44 | 0.90 |
2.0001 | 7.97 | |||
2.0003 | 8.03 | |||
S5 | 2.0002 | 9.17 | 9.19 | 0.31 |
2.0001 | 9.17 | |||
2.0000 | 9.22 | |||
S6 | 2.0002 | 7.64 | 7.68 | 0.69 |
2.0000 | 7.66 | |||
1.9999 | 7.74 | |||
S7 | 1.9999 | 8.36 | 8.39 | 0.36 |
2.0000 | 8.38 | |||
2.0000 | 8.42 | |||
S8 | 2.0000 | 8.06 | 8.07 | 0.38 |
2.0002 | 8.04 | |||
2.0000 | 8.10 | |||
S9 | 1.9999 | 8.79 | 8.86 | 0.79 |
1.9999 | 8.93 | |||
2.0000 | 8.87 | |||
S10 | 1.9998 | 8.36 | 8.46 | 1.13 |
1.9998 | 8.47 | |||
2.0000 | 8.55 | |||
S11 | 2.0002 | 9.21 | 9.30 | 0.88 |
2.0001 | 9.32 | |||
1.9997 | 9.37 | |||
S12 | 2.0000 | 8.26 | 8.27 | 0.67 |
2.0000 | 8.33 | |||
2.0002 | 8.22 | |||
S13 | 1.9997 | 7.96 | 7.92 | 0.58 |
1.9998 | 7.93 | |||
2.0001 | 7.87 | |||
S14 | 2.0000 | 8.93 | 8.87 | 0.68 |
2.0000 | 8.81 | |||
1.9998 | 8.88 | |||
S15 | 1.9997 | 8.69 | 8.68 | 0.42 |
1.9999 | 8.71 | |||
1.9997 | 8.64 | |||
S16 | 2.0001 | 7.99 | 8.05 | 1.11 |
2.0000 | 8.00 | |||
1.9997 | 8.15 | |||
S17 | 2.0001 | 8.30 | 8.34 | 0.55 |
2.0001 | 8.39 | |||
1.9998 | 8.33 | |||
S18 | 2.0000 | 9.34 | 9.37 | 0.38 |
1.9999 | 9.33 | |||
1.9997 | 9.39 | |||
S19 | 2.0002 | 8.53 | 8.54 | 0.49 |
2.0003 | 8.51 | |||
2.0002 | 8.59 | |||
S20 | 2.0003 | 7.99 | 7.95 | 0.67 |
2.0001 | 7.89 | |||
2.0000 | 7.97 | |||
S21 | 2.0000 | 7.77 | 7.81 | 0.75 |
2.0000 | 7.88 | |||
1.9998 | 7.79 | |||
S22 | 1.9999 | 8.40 | 8.43 | 0.49 |
2.0000 | 8.42 | |||
2.0003 | 8.48 | |||
S23 | 2.0000 | 8.65 | 8.69 | 1.04 |
2.0003 | 8.62 | |||
2.0001 | 8.79 | |||
S24 | 1.9997 | 7.95 | 7.93 | 0.84 |
1.9999 | 7.86 | |||
2.0001 | 7.99 |
表4. 马蓝水分含量测定结果(n = 3)
由表4可知,马蓝水分含量7.68%~9.37%。马蓝平均水分含量为8.39%,其中S18的水分含量最高为9.37%,S6的水分含量最低为7.68%。
批次 | 取样量(g) | 总灰分(%) | 平均值(%) | RSD(%) | |||||
---|---|---|---|---|---|---|---|---|---|
S1 | 5.0002 | 9.29 | 9.32 | 0.53 | |||||
5.0000 | 9.38 | ||||||||
5.0001 | 9.30 | ||||||||
S2 | 4.9998 | 9.98 | 9.94 | 0.73 | |||||
5.0000 | 9.86 | ||||||||
5.0001 | 9.99 | ||||||||
S3 | 5.0002 | 7.32 | 7.32 | 0.89 | |||||
4.9999 | 7.26 | ||||||||
5.0000 | 7.39 | ||||||||
S4 | 4.9998 | 7.71 | 7.75 | 0.52 | |||||
5.0001 | 7.75 | ||||||||
5.0002 | 7.79 | ||||||||
S5 | 5.0001 | 9.82 | 9.81 | 0.57 | |||||
5.0002 | 9.86 | ||||||||
5.0001 | 9.75 | ||||||||
S6 | 5.0000 | 9.11 | 9.15 | 0.58 | |||||
5.0000 | 9.21 | ||||||||
4.9999 | 9.13 | ||||||||
S7 | 5.0000 | 8.72 | 8.77 | 0.83 | |||||
5.0001 | 8.73 | ||||||||
4.9997 | 8.80 | ||||||||
S8 | 5.0002 | 9.01 | 9.09 | 1.02 | |||||
5.0001 | 9.06 | ||||||||
5.0002 | 9.19 | ||||||||
S9 | 5.0000 | 8.08 | 8.08 | 0.68 | |||||
5.0001 | 8.02 | ||||||||
4.9999 | 8.13 | ||||||||
S10 | 5.0000 | 9.24 | 9.25 | 0.35 | |||||
4.9999 | 9.29 | ||||||||
4.9997 | 9.23 | ||||||||
S11 | 5.0001 | 9.64 | 9.65 | 0.33 | |||||
4.9999 | 9.69 | ||||||||
4.9998 | 9.63 | ||||||||
S12 | 5.0000 | 7.36 | 7.36 | 0.61 | |||||
5.0000 | 7.40 | ||||||||
5.0003 | 7.31 | ||||||||
S13 | 5.0000 | 8.92 | 8.93 | 0.57 | |||||
5.0002 | 8.99 | ||||||||
4.9998 | 8.89 | ||||||||
S14 | 5.0000 | 8.09 | 8.08 | 0.87 | |||||
5.0000 | 8.06 | ||||||||
5.0003 | 8.15 | ||||||||
S15 | 5.0002 | 8.90 | 8.87 | 1.13 | |||||
5.0000 | 8.77 | ||||||||
4.9999 | 8.87 | ||||||||
S16 | 5.0002 | 8.63 | 8.65 | 0.44 | |||||
5.0001 | 8.62 | ||||||||
4.9998 | 8.69 | ||||||||
S17 | 5.0000 | 9.84 | 9.85 | 0.41 | |||||
5.0000 | 9.89 | ||||||||
5.0002 | 9.81 | ||||||||
S18 | 5.0001 | 9.56 | 9.56 | 0.37 | |||||
5.0002 | 9.59 | ||||||||
5.0002 | 9.52 | ||||||||
S19 | 4.9998 | 8.31 | 8.34 | 0.43 | |||||
5.0000 | 8.33 | ||||||||
4.9999 | 8.38 | ||||||||
S20 | 5.0000 | 8.95 | 8.95 | 0.45 | |||||
5.0000 | 8.91 | ||||||||
5.0002 | 8.99 | ||||||||
S21 | 5.0000 | 7.68 | 7.74 | 0.78 | |||||
5.0001 | 7.80 | ||||||||
4.9999 | 7.73 | ||||||||
S22 | 5.0001 | 8.39 | 8.38 | 0.96 | |||||
5.0000 | 8.29 | ||||||||
4.9997 | 8.45 | ||||||||
S23 | 5.0001 | 8.86 | 8.88 | 0.60 | |||||
5.0002 | 8.94 | ||||||||
4.9998 | 8.84 | ||||||||
S24 | 4.9999 | 8.02 | 8.08 | 0.82 | |||||
5.0001 | 8.15 | ||||||||
5.0002 | 8.06 | ||||||||
表5. 马蓝总灰分测定结果(n = 3)
批次 | 酸不溶灰分(%) | 平均值(%) | RSD(%) |
---|---|---|---|
S1 | 1.04 | 1.03 | 0.97 |
1.02 | |||
1.03 | |||
S2 | 0.74 | 0.74 | 0.78 |
0.73 | |||
0.74 | |||
S3 | 0.55 | 0.55 | 1.04 |
0.56 | |||
0.55 | |||
S4 | 0.85 | 0.85 | 1.80 |
0.83 | |||
0.86 | |||
S5 | 0.92 | 0.91 | 1.10 |
0.90 | |||
0.91 | |||
S6 | 0.79 | 0.79 | 0.73 |
0.80 | |||
0.79 | |||
S7 | 0.65 | 0.66 | 1.74 |
0.67 | |||
0.67 | |||
S8 | 0.69 | 0.68 | 1.69 |
0.67 | |||
0.69 | |||
S9 | 0.62 | 0.62 | 0.93 |
0.62 | |||
0.63 | |||
S10 | 1.06 | 1.07 | 1.08 |
1.08 | |||
1.08 | |||
S11 | 0.68 | 0.70 | 2.99 |
0.72 | |||
0.69 | |||
S12 | 0.71 | 0.71 | 0.81 |
0.71 | |||
0.72 | |||
S13 | 0.97 | 0.96 | 1.20 |
0.97 | |||
0.95 | |||
S14 | 0.75 | 0.74 | 0.78 |
0.74 | |||
0.74 | |||
S15 | 0.64 | 0.63 | 0.91 |
0.63 | |||
0.63 | |||
S16 | 0.76 | 0.77 | 1.98 |
0.77 | |||
0.79 | |||
S17 | 0.93 | 0.95 | 1.82 |
0.96 | |||
0.96 | |||
S18 | 0.97 | 0.96 | 0.60 |
0.96 | |||
0.96 | |||
S19 | 0.51 | 0.51 | 1.14 |
0.51 | |||
0.50 | |||
S20 | 0.84 | 0.84 | 0.68 |
0.85 | |||
0.84 | |||
S21 | 0.95 | 0.95 | 0.61 |
0.95 | |||
0.96 | |||
S22 | 0.73 | 0.73 | 2.08 |
0.72 | |||
0.75 | |||
S23 | 0.88 | 0.87 | 0.66 |
0.87 | |||
0.87 | |||
S24 | 1.04 | 1.02 | 1.96 |
1.00 | |||
1.02 |
表6. 马蓝酸不溶灰分测定结果(n = 3)
按照2020年版《中国药典》第四部2303灰分测定法中的总灰分测定法测定( [
由表5可知,马蓝总灰分含量7.32%~9.94%,马蓝平均总灰分含量为8.74%。其中S2的总灰分含量最高为9.94%,S3的总灰分含量最低为7.32%。
由表6可知,马蓝酸不溶灰分含量0.51%~1.01%,酸不溶灰分平均含量为0.80%,其中S1的酸不溶含量最高为1.01%,S19的酸不溶含量最低为7.32%,低于其平均含量。酸不溶灰分可以反应药材泥土砂石等杂质的掺杂量,因此酸不溶灰分对药材的纯度有影响,建议马蓝的酸不溶灰分不得超过3.0%。
批次 | 取样量(g) | 浸出物(%) | 平均值(%) | RSD (%) |
---|---|---|---|---|
S1 | 3.0000 | 14.45 | 14.46 | 0.80 |
3.0000 | 14.35 | |||
3.0002 | 14.58 | |||
S2 | 3.0001 | 16.81 | 16.65 | 0.96 |
3.0000 | 16.49 | |||
2.9998 | 16.66 | |||
S3 | 2.9999 | 16.88 | 16.81 | 1.19 |
3.0000 | 16.98 | |||
3.0001 | 16.90 | |||
S4 | 3.0000 | 15.80 | 15.64 | 1.25 |
3.0001 | 15.42 | |||
2.9997 | 15.69 | |||
S5 | 3.0001 | 22.36 | 22.40 | 0.60 |
3.0001 | 22.29 | |||
2.9998 | 22.31 | |||
S6 | 3.0001 | 24.55 | 24.58 | 1.30 |
3.0000 | 24.48 | |||
3.0003 | 24.59 | |||
S7 | 3.0000 | 26.25 | 26.13 | 0.44 |
3.0000 | 26.02 | |||
3.0002 | 26.13 | |||
S8 | 3.0000 | 26.58 | 26.27 | 1.02 |
3.0001 | 26.15 | |||
2.9999 | 26.09 | |||
S9 | 2.9999 | 25.79 | 25.66 | 0.53 |
2.9999 | 25.66 | |||
2.9997 | 25.52 | |||
S10 | 3.0000 | 26.84 | 26.76 | 0.40 |
2.9999 | 26.64 | |||
2.9998 | 26.81 | |||
S11 | 3.0000 | 17.98 | 17.94 | 0.47 |
3.0000 | 17.84 | |||
3.0003 | 17.99 | |||
S12 | 3.0001 | 17.88 | 17.72 | 0.97 |
3.0000 | 17.75 | |||
3.0002 | 17.54 | |||
S13 | 3.0000 | 15.48 | 15.37 | 0.72 |
3.0001 | 15.38 | |||
2.9999 | 15.26 | |||
S14 | 3.0001 | 15.69 | 15.70 | 0.51 |
3.0000 | 15.62 | |||
2.9997 | 15.78 | |||
S15 | 3.0001 | 18.66 | 18.47 | 1.09 |
3.0000 | 18.49 | |||
2.9999 | 18.26 | |||
S16 | 3.0000 | 14.73 | 14.64 | 0.59 |
3.0000 | 14.62 | |||
3.0003 | 14.56 | |||
S17 | 2.9999 | 14.81 | 14.89 | 0.50 |
3.0001 | 14.89 | |||
3.0003 | 14.96 | |||
S18 | 3.0000 | 20.74 | 20.43 | 1.62 |
3.0001 | 20.70 | |||
3.0000 | 20.79 | |||
S19 | 3.0002 | 18.91 | 18.88 | 0.62 |
3.0001 | 18.98 | |||
2.9997 | 18.75 | |||
S20 | 3.0000 | 17.63 | 17.41 | 1.54 |
3.0000 | 17.48 | |||
2.9998 | 17.11 | |||
S21 | 3.0000 | 16.55 | 16.52 | 0.46 |
2.9999 | 16.57 | |||
2.9998 | 16.43 | |||
S22 | 3.0001 | 20.07 | 20.16 | 0.86 |
3.0000 | 20.35 | |||
3.0003 | 20.12 | |||
S23 | 3.0001 | 18.61 | 18.49 | 0.89 |
3.0000 | 18.49 | |||
3.0002 | 18.55 | |||
S24 | 3.0000 | 17.55 | 17.52 | 0.51 |
3.0001 | 17.59 |
表7. 马蓝浸出物含量测定结果(n = 3)
按照2020年版《中国药典》第四部2201醇溶性浸出物测定法的热浸法进行测定( [
由表7可知,马蓝浸出物含量14.46%~26.76%,马蓝平均浸出物含量为19.15%,其中S10的浸出物含量最高为26.76%,S1的浸出物含量最低为14.46%。
中药储存过程中,药材含水量是影响其质量的关键指标之一,药材水分过高,不但会影响药材外观性状,而且还会导致霉变、虫蛀等现象 [
本研究对马蓝药材进行了水分、总灰分、酸不溶性灰分及浸出物含量的测定,为马蓝药材质量标准的建立提供了数据支撑。根据实验结果并参考2020版《中国药典》中南板蓝根的相关规定,建议马蓝药材的水分暂定不超过12%,总灰分不超过10%,酸不溶性灰分不超过3%,浸出物不少于10%。
贵州中医药大学校企合作项目(榕江县马蓝产业科技创新关键技术协作攻关,编号:2021-3-01)。
杨武海,黄子涵,于 浩,杨 烨,吴之坤. 马蓝药材中水分、灰分及浸出物的测定Determination of Moisture, Ash and Extract in Strobilanthes cusia[J]. 药物资讯, 2024, 13(03): 270-281. https://doi.org/10.12677/pi.2024.133032