以微波消化法和灰化法分析中藥材內所含鉛、銅、鎘之重金屬

The analysis of heavy metal content such as lead, copper, and cadmium in traditional Chinese medicine with microwave digestion method and ash method

洪盈鈴(YING-LING HUNG)

指導教授 ： 謝博進

中原大學/理學院/化學系/碩士(2008年)

https://doi.org/10.6840/cycu200900069

摘要

摘 要
中藥材的品質管制，目前尚未有完整的規定，大部分的藥廠是自行參考各國藥典，制定廠規來控管品質。在這些檢驗規格中，對於個別中藥材重金屬的分析規範不多，目前一般主要用比色法來檢測總鉛含量，其餘的金屬並沒有強制規定需檢驗。目前在國內台灣傳統藥典（the Taiwanese Herbal Pharmacopoeia）所收載的藥材中，只對少數藥材之規範，其餘至今仍在討論。為保障民眾用藥安全與藥廠藥材之品質改善，對中藥材重金屬的探討與研究有其必要性。
實驗所用之中藥材購自國內中藥貿易商或藥商，中藥材可分成植物、動物、礦物三大類，其中植物類又分成花朵、果實、種子、根、莖、皮、葉、全草等八類。因為中藥材是固態樣品種類多，可用不同的前處理法來比較其差異性，分析前需先用灰化法和微波消化法將樣品消化後，用不同儀器商所製造之火焰原子吸收光譜儀來進行化驗比較其差異性。
由實驗結果得到紅棗(植物類)用灰化法消化其樣品回收率(Sample recovery) 為62.3- 70.2 %，石決明(礦物類) 為 5.3 -5.5%，蟬蛻(動物類)率為58.5 - 77.8 %。紅棗用微波消化法消化其樣品回收率為103.6 -103.7 %，石決明為94.5- 101.1 %，蟬蛻為104.6 – 110.7 %。由結果得知在樣品前處理法的比較中，微波消化法較適用。
此次檢驗所得到之數據中，珍珠粉（1）、珍珠粉（2）、雄黃、石決明、石膏等礦物類的鉛和鎘用微波消化法完成後，使用不同儀器廠商之火焰原子吸收光譜儀檢測，用方法II (PE AA3300 微波消化法)消化鉛元素波長用283.3 nm檢測其結果分別是50.632 ppm、49.584 ppm、10.968 ppm、50.405 ppm、17.237 ppm，用方法IV (Varian AA280 微波消化法)消化鉛元素波長用283.3 nm檢測其結果分別是15.452 ppm、8.325 ppm、7.625 ppm、9.446 ppm、2.589 ppm，用方法II消化檢測鎘元素其結果分別是2.912 ppm、2.814 ppm、1.415 ppm、2.129 ppm、1.038 ppm，用方法IV消化檢測鎘元素其結果分別是0.056 ppm、0.104 pm、0.209 ppm、0.102 ppm、0.047 ppm，由結果得知兩種方法其差異過大，需留待日後能進一步的研究確認。但鉛元素用217.0 nm波長檢測，數據變化大，大部份的中藥材其相對標準偏差（RSD）大於100 % 以上，表示此波長不適合當中藥材的偵測光譜。

關鍵字

中藥材 ； 重金屬 ； 原子吸收光譜儀 ； 灰化法 ； 微波消化法

並列摘要

Abstract
The quality control (QC) of traditional Chinese medicine has not yet established a universal standard. Most pharmaceutical factories refer to various foreign stipulations to formulate their own quality control protocols, which have not done much to regulate the heavy metal content in different kinds of traditional Chinese medicine. Pharmaceutical factories use colorimetry to examine lead in Chinese medicine, but these factories are not enforced to inspect other heavy metal content.
Though the Taiwanese Herbal Pharmacopoeia has established inspection standards, they are for limited raw material, not for all Chinese medicine. In order to protect general users’ use safety of Chinese medicine and to set universal standards to improve quality control, it is necessary to research and regulate the heavy metals content in Chinese medicine.
The research approach to experimental analysis is to purchase traditional Chinese medicine from domestic traders or apothecaries. The traditional Chinese medicine is mainly divided into three categories— Plant, animal, and mineral. The category of plant includes flower, fruit, seed, root, stem, bark, leaf, and grass. In general, since various types of traditional Chinese medicine are solid, they could be processed by different pre-processing methods to compare the differenences. Before the analysis, Dry Ash method and Microwave Digestion methods need to be used to digest testing samples, and then use flame atom absorption spectroscopes made by different instrumental manufacturers to do the chemical examinations.
The result of this experiment is obtaining Fructus Jujubae(plant category) that digests 62.3-70.2% sample recovery with the Ash method, the Concha Haliotidis (mineral category) is 5.3 -5.5%, the cicada slough (animal category) rate is 58.5 - 77.8%. The Fructus Jujubae that digests its sample recovery with the microwave digestion method is 103.6 -103.7%, the Concha Haliotidis is 94.5- 101.1%, the cicada slough is 104.6 - 110.7%. By comparing the results from different pre-processing methods, Microwave Digestion method is better.
After the completion of lead and cadmium in the minerals like Margarita (1)
、Margarita (2)、 Realgar 、Concha Haliotidis、Gypsum Fibrosum by the
microwave digestion method, and then use different flame atom absorption
spectroscopes (AA) to do the examination, the data shows that by using method II (PE AA3300 microwave digestion method) digestion and the lead element with 283.3 nm wave length, the result of the examination is respectively 50.632 ppm, 49.584 ppm, 10.968 ppm, 50.405 ppm, 17.237 ppm; by using method IV
(Varian AA280 microwave digestion method) digestion and the lead element with 283.3 nm wave length, the result of the examination is respectively 15.452 ppm, 8.325 ppm, 7.625 ppm, 9.446 ppm, 2.589 ppm; by using method II digestion and cadmium element, the result of the examination is respectively 2.912 ppm, 2.814 ppm, 1.415 ppm, 2.129 ppm, 1.038 ppm; by using method IV digestion and cadmium element, the result of the examination is respectively 0.056 ppm, 0.104 pm, 0.209 ppm, 0.102 ppm, 0.047 ppm. According to the result, the differences of the two methods are oversized, so we have to wait until further research confirmation in the future. However, by using lead under 217.0 nm wave length to do the examination, the collected data are very different, and the relatively standard deviation (RDS) of most traditional Chinese medicine is above 100%. Thus, we can make the conclusion that this wave length is not suitable to be used for traditional Chinese medicine detection spectrum.

並列關鍵字

Flame atom absorption spectroscopes ； traditional Chinese medicine ； heavy metal ； Ash method ； Microwave Digestion method

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