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CN103512848B - A kind of Rhizoma Coptidis colourity digitlization quality detecting method and equipment thereof - Google Patents

A kind of Rhizoma Coptidis colourity digitlization quality detecting method and equipment thereof Download PDF

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CN103512848B
CN103512848B CN201310201173.5A CN201310201173A CN103512848B CN 103512848 B CN103512848 B CN 103512848B CN 201310201173 A CN201310201173 A CN 201310201173A CN 103512848 B CN103512848 B CN 103512848B
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coptis chinensis
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rhizoma coptidis
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CN103512848A (en
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吉光见稚代
瞿显友
王昌华
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Chongqing Academy of Chinese Materia Medica
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Abstract

本发明提供了一种黄连药材色度数字化品质检测方法,包括以下步骤:1)将黄连药材粉碎,得到黄连粉末;2)将黄连粉末置于比色皿中,采用刺激值直读法或分光测色法测定出三刺激值X、Y、Z;3)将三刺激值X、Y、Z计算给出<i>L*,a*,b*</i>;4)通过<i>L*,a*,b*</i>在坐标系中的位置判断黄连药材的品种及品质;各黄连品种有特色的生物碱组成,生物碱组成及含量反映黄连色度。因此,黄连的色度可以容易区别黄连品种,可以判断味连的品质。该方法为中药材品质品价的一种新的方法。

The invention provides a digital quality detection method for chroma of Coptidis medicinal material, comprising the following steps: 1) crushing Coptidis medicinal material to obtain Coptidis rhizome powder; Three stimulus values X, Y, Z are determined by colorimetry; 3) Calculate the three stimulus values X, Y, Z to give <i>L * , a * , b * </i>; 4) Pass <i> The position of L * , a * , b * </i> in the coordinate system can be used to determine the variety and quality of Coptis chinensis; each Coptis chinensis variety has a characteristic alkaloid composition, and the alkaloid composition and content reflect the color of Coptis chinensis. Therefore, the chroma of Coptis chinensis can easily distinguish Coptis chinensis species, and can judge the quality of Milian. This method is a new method for the quality and price of Chinese medicinal materials.

Description

一种黄连药材色度数字化品质检测方法及其设备A digital chromaticity quality detection method and equipment for Coptis chinensis medicinal material

技术领域technical field

本发明涉及一种中药材检测设备及其检测方法,更具体的说涉及一种黄连药材色度数字品质检测方法及其设备。The invention relates to a Chinese medicinal material detection device and a detection method thereof, and more specifically relates to a chromaticity digital quality detection method of Coptis chinensis medicinal material and the detection method thereof.

技术背景technical background

黄连为毛茛科植物CoptischinensisFranch.、三角叶黄连CoptisdeltoideaC.Y.ChengetHsiao或云连Coptisteetawall.的干燥根茎,始载于东汉《神农本草经》,列为上品,具有泻火解毒、清热燥湿等功效。《中国药典》2010年版记载性状,表面灰黄色或黄褐色,皮部橙红色或暗棕色,木部鲜黄色或橙黄色。记载成分含量,按干燥品计算,以盐酸小檗碱计,含小檗碱不得少于5.5%,表小檗碱不得少于0.80%,黄连碱不得少于1.6%,巴马汀不得少于1.5%。还有《集注本草》记载了建平产黄连,颜色浅虚不用。古代中药材颜色是一个使用的判断基准。Coptis chinense is the dried rhizome of Coptischinensis Franch., Coptis deltoidea C.Y. Chenget Hsiao or Coptisteetawall. Coptis deltoidea C.Y. Chenget Hsiao of Ranunculaceae. "Chinese Pharmacopoeia" 2010 edition records the traits, the surface is grayish yellow or yellowish brown, the skin is orange red or dark brown, and the xylem is bright yellow or orange yellow. The content of recorded ingredients is calculated on the basis of dry products, calculated as berberine hydrochloride, containing not less than 5.5% berberine, not less than 0.80% epiberberine, not less than 1.6% coptisine, and not less than palmatine 1.5%. There is also "Jizhu Materia Medica" which records that Jianping produces Coptis chinensis, which is light in color and not used. The color of ancient Chinese herbal medicines is a criterion used for judging.

近代,与色、光相关的国际性协商机构—国际标准化团体:组建了国际照明委员会(CIE:CommissionInternationaldeI‘Eclairege)。CIE于1931年制定“XYZ(Yxy)表色系统”、1976年制定“L*a*b*表色系统(CIE1976Lab表色系统)”。采用这些表色系统使全球用统一的色度表示成为可能。In modern times, an international consultative body related to color and light—the international standardization group: the International Commission on Illumination (CIE: Commission International de I'Eclairege) was established. CIE formulated the "XYZ (Yxy) Color System" in 1931 and the "L*a*b* Color System (CIE1976Lab Color System)" in 1976. The adoption of these colorimetric systems has made it possible to express uniform chromaticity globally.

目前目测法最为常用,成本低,操作简便,但这一方法仅仅凭借实验者的感官判断药品质量,容易受实验者主观的影响,故不够科学严谨;紫外-可见分光光度法通常选择在某一特定波长处测定药品溶液颜色,而实际上,中药制剂成分复杂,药品溶液的颜色是不同波长共同作用的结果,故单单凭借一特定波长吸光值无法准确反映药品溶液颜色;色差仪测定药品溶液颜色通过依托CIELab色空间,用CIELab三维坐标中一个特定的点来表示某一特定的颜色,这一方法操作简便,准确度高,判断精准。At present, the visual method is the most commonly used method, which is low in cost and easy to operate. However, this method only relies on the experimenter's sense to judge the quality of the drug, which is easily affected by the experimenter's subjectivity, so it is not scientific and rigorous; UV-visible spectrophotometry is usually selected in a certain The color of the drug solution is measured at a specific wavelength. In fact, the composition of traditional Chinese medicine preparations is complex, and the color of the drug solution is the result of the joint action of different wavelengths. Therefore, the color of the drug solution cannot be accurately reflected only by the absorbance value of a specific wavelength; the color difference meter measures the color of the drug solution. Relying on the CIELab color space, a specific point in the CIELab three-dimensional coordinates is used to represent a specific color. This method is easy to operate, high in accuracy, and precise in judgment.

发明内容Contents of the invention

为解决上述问题,本发明提供了一种黄连药材色度数字化品质检测设备,所述检测设备包括测色仪、光源和比色皿;其中比色皿置于恒温装置中。In order to solve the above problems, the present invention provides a chromaticity digital quality detection device for Coptis rhizome medicinal material. The detection device includes a colorimeter, a light source and a cuvette; wherein the cuvette is placed in a constant temperature device.

所述光源为标准A光,C光,D65光,D50光,ID65光,ID50光,F2,F6,F7,F8,F10光,F11,F12中的一种光源,照明方式为扩散照明,反射光;所述测色仪的观察视野:2°及10°。The light source is one of standard A light, C light, D65 light, D50 light, ID65 light, ID50 light, F2, F6, F7, F8, F10 light, F11, F12, and the lighting method is diffuse lighting, reflection Light; the observation field of view of the colorimeter: 2° and 10°.

一种黄连药材色度数字化品质检测方法,包括以下步骤:A chromatic digital quality detection method for Coptis rhizome medicinal material, comprising the following steps:

1)将黄连药材粉碎,得到黄连粉末;1) Pulverizing Coptidis Rhizoma to obtain Coptidis Rhizoma powder;

2)将黄连粉末置于比色皿中,采用刺激值直读法或分光测色法测定出三刺激值X、Y、Z;2) Put the Coptidis rhizome powder in a cuvette, and measure the three stimulus values X, Y, Z by direct reading method or spectrophotometry;

3)将三刺激值X、Y、Z计算给出L*,a*,b*3) Calculate the tristimulus values X, Y, and Z to give L * , a * , b * ;

4)通过L*,a*,b*在坐标系中的位置判断黄连药材的品种及品质。4) Judging the variety and quality of Coptis chinensis by the position of L * , a * , b * in the coordinate system.

步骤4)通过读取L*,a*,b*的值,判断黄连总生物碱含量。Step 4) Determine the total alkaloid content of Coptidis Rhizoma by reading the values of L * , a * and b * .

步骤4)通过判断a*,b*的在坐标系中的位置区间,判断黄连的品种。Step 4) By judging the position interval of a * and b * in the coordinate system, the variety of Coptis chinensis is judged.

本发明的有益技术效果是:各黄连品种有特色的生物碱组成,生物碱组成及含量反映黄连色度。因此,黄连的色度可以容易区别黄连品种,可以判断味连的品质。该方法为中药材品质品价的一种新的方法。特别有效对饮片中药,粉末中药。该方法,操作简单、缩短时间,低成本、可行广泛普及,可作为黄连药材质量品价依据。展开更多的中药材、又可以应用加工工程管理等。The beneficial technical effects of the present invention are: each Coptis chinensis variety has characteristic alkaloid composition, and the alkaloid composition and content reflect the chroma of Coptis chinensis. Therefore, the chroma of Coptis chinensis can easily distinguish Coptis chinensis species, and can judge the quality of Milian. This method is a new method for the quality and price of Chinese medicinal materials. Especially effective for sliced Chinese medicine and powdered Chinese medicine. The method has the advantages of simple operation, shortened time, low cost, feasibility and widespread popularization, and can be used as the basis for the quality and price of Coptis chinensis medicinal materials. Expand more Chinese medicinal materials, and can also apply processing engineering management.

附图说明Description of drawings

图1味连,雅连,云连及日本黄连的色相在二位坐标系中的位置区间;Figure 1 The position interval of the hue of Milian, Yalian, Yunlian and Coptis chinensis in the two-dimensional coordinate system;

图2味连中色相(a*)与小檗碱含量的关系。Fig. 2 Relationship between hue (a * ) and berberine content in Milian.

具体实施方式detailed description

实施例1黄连药材色度数字品质检测方法对黄连药材品种的检测方法考察Example 1 Investigation of Coptis Rhizoma Varieties by Colorimetric Digital Quality Detection Method of Coptis Rhizoma

从市场上采购各品种的黄连药材;具体如表1所示;Purchase the Coptis chinensis medicinal materials of various varieties from the market; specifically as shown in Table 1;

表1实验药材Table 1 Experimental Medicinal Materials

市场买的商品黄连,先60℃以下8个小时以上干燥,然后先附编码(CQMY),在重庆市中药研究院保存所有的实验药材。Coptis chinensis bought in the market is first dried at 60°C for more than 8 hours, and then coded (CQMY), and all experimental medicinal materials are stored in Chongqing Academy of Traditional Chinese Medicine.

采用黄连药材色度数字品质检测方法测定中药粉末的反射光,采用HPLC方法定量黄连的6个生物碱含量。The reflected light of traditional Chinese medicine powder was measured by chromaticity digital quality detection method of Coptidis rhizome, and the content of six alkaloids in Coptidis rhizome was quantified by HPLC method.

1、采用黄连药材色度数字品质检测方法测定中药粉末的反射光1. Determination of reflected light of traditional Chinese medicine powder by chromaticity digital quality detection method of Coptis chinensis

条件扩散照明(积分球)方式;反射光;光源:标准A光,C光,D65光,D50光,ID65光,ID50光,F2,F6,F7,F8,F10光,F11,F12;观察视野:2°及10°;表色系:CIEL*a*b*表色系(CIE);分光反射率:360nm~740nm;专用比色皿12mm*10mm;测定値:采用5次测定后的平均値。尚,L*a*b*表色系是,在360nm~740波长分解物体反射的光,在按照一定的规律,并转换为3个数字L*a*b*,L*(0.00-100.00)是代表明度,a*及b*代表色相。Conditional diffuse lighting (integrating sphere) mode; reflected light; light source: standard A light, C light, D65 light, D50 light, ID65 light, ID50 light, F2, F6, F7, F8, F10 light, F11, F12; observation field of view : 2° and 10°; color system: CIEL*a*b* color system (CIE); spectral reflectance: 360nm~740nm; special cuvette 12mm*10mm; measurement value: the average after 5 measurements value. Still, the L*a*b* color system is to decompose the light reflected by the object at a wavelength of 360nm~740, and convert it into three numbers according to certain rules. L*a*b*, L*(0.00-100.00) is the lightness, a* and b* the hue.

测定条件是0/d或d/0,D65光源照明,10°视场,可直接测出三刺激X,Y,Z并能直接计算给出L*,a*,b*和ΔE*及样品的色调色号。在本研究对粉末测定考虑了观察条件13个光源及2个视场:10°与2°品种之间的区别C光源照明,2°视场观察条件最明显,味连平均a*值10.31±1.43,b*值53.36±6.85,雅连a*值8.89、9.39,b*33.32、33.34、云连a*值5.17、b*值46.69,另外日本黄连色相类似云连,具体结论见表2所示。The measurement condition is 0/d or d/0, D65 light source illumination, 10° field of view, can directly measure the tristimulus X, Y, Z and can directly calculate and give L*, a*, b* and ΔE* and samples The color shade number. In this study, 13 light sources and 2 fields of view were considered for the determination of powder: the difference between 10° and 2° varieties of C light source illumination, the observation condition of 2° field of view is the most obvious, and the average a* value of Milian is 10.31± 1.43, b* value 53.36±6.85, Yalian a* value 8.89, 9.39, b* 33.32, 33.34, Yunlian a* value 5.17, b* value 46.69, and the color of Coptis chinensis is similar to Yunlian, the specific conclusion is shown in Table 2 Show.

表2.不同照射光L*a*b*值Table 2. L*a*b* value of different irradiation light

所有药材的色相a*,b*标注在二位坐标系中,具体如图1所示。三个品种中云连是a*值极低、雅連是b*值显著低。因此,色相a*及b*可以区别味连和云连,雅连。The hue a* and b* of all medicinal materials are marked in the two-dimensional coordinate system, as shown in Figure 1. Among the three varieties, the a* value of Yunlian was extremely low, and the b* value of Yalian was significantly low. Therefore, the hues a* and b* can distinguish Milian from Yunlian and Yalian.

实施例2黄连药材色度数字品质检测方法对黄连药材品质测定方法的考察Example 2 Investigation of Coptis Rhizoma Medicinal Material Chromaticity Digital Quality Detection Method on Coptis Rhizoma Medicinal Material Quality Determination Method

1、HPLC方法测定生物碱含量1. Determination of alkaloid content by HPLC method

采用HPLC法测定3份的平均值。The average value of 3 copies was determined by HPLC method.

恒量的干燥粉末(过三号筛)搅拌混合、取本品粉末約0.5g。A constant amount of dry powder (passed through a No. 3 sieve) is stirred and mixed, and about 0.5g of the powder of this product is taken.

对照品溶液的制备取药根碱、非洲防己碱、表小檗碱、黄连碱、巴马汀及小檗碱对照品各适量,甲醇溶解定容,制成浓度分别为22.1、19.5、65.6、93.8、59.4及302.8ug/ml的混合对照品溶液。Preparation of Reference Substance Solution Take appropriate amounts of jatrorrhizine, african tetrandrine, epiberberine, coptisine, palmatine and berberine reference substances, dissolve in methanol to constant volume, and make concentrations of 22.1, 19.5, 65.6, 93.8, 59.4 and 302.8ug/ml mixed reference solution.

供试品溶液的制备取本品粉末约0.2g(3份),精密称定,置具塞锥形瓶中,精密加入甲醇-盐酸(100:1)的混合溶液50ml,密塞,称定重量,超声处理(功率250W,频率40kHz)30min,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过,精密量取续滤液2ml,置10ml量瓶中,加甲醇至刻度,摇匀,滤过,取续滤液,即得。Preparation of the test solution Take about 0.2g (3 parts) of the powder of this product, weigh it accurately, put it in a stoppered Erlenmeyer flask, accurately add 50ml of methanol-hydrochloric acid (100:1) mixed solution, seal it tightly, and weigh it. Weight, ultrasonic treatment (power 250W, frequency 40kHz) for 30min, let cool, weigh again, make up for the lost weight with methanol, shake well, filter, accurately measure the filtrate 2ml, put it in a 10ml measuring bottle, add methanol To the mark, shake well, filter, take the continued filtrate, that is.

仪器LC-20A(日本岛津),紫外检测器。色谱条件采用YMC-TriartC18色谱柱(250mm×4.6mm,5μm);检测波长为270nm;流动相为乙腈A-0.1mol/L乙酸铵B(梯度洗脱,见表1;0.1mol/L乙酸铵以氨水调PH值至9.5);流速为1mL·min-1;柱温为30℃。理论板数应不低于5×103,洗脱条件如表3所示;检测实施例1中各黄连药材样品药根碱、非洲防己碱、表小檗碱、黄连碱、巴马汀及小檗碱的含量。Instrument LC-20A (Shimadzu, Japan), UV detector. The chromatographic conditions adopt YMC-TriartC 18 chromatographic column (250mm×4.6mm, 5μm); the detection wavelength is 270nm; the mobile phase is acetonitrile A-0.1mol/L ammonium acetate B (gradient elution, see Table 1; 0.1mol/L acetic acid Ammonium was used to adjust the pH value to 9.5 with ammonia water); the flow rate was 1mL·min -1 ; the column temperature was 30°C. The number of theoretical plates should not be less than 5×10 3 , and the elution conditions are shown in Table 3; the jatrorrhizine, africa tetrandrine, epiberberine, coptisine, palmatine and Berberine content.

表3梯度洗脱程序Table 3 Gradient elution program

2、结合实施例1得到的各个黄连药材中的L*a*b*值和本实施例得到各黄连药材中黄连主要生物碱的含量数据研究发现。2. Combining the L*a*b* values in each Coptidis medicinal material obtained in Example 1 with the content data of Coptidis major alkaloids in each Coptidis medicinal material obtained in this example.

云连及日本黄连比味连6个生物碱中非洲防己碱、巴马汀,表小檗碱含量极端少、药根碱含量比较高,具体结果见表4所示。Among the 6 alkaloids in Yunlian and Coptis chinensis than Milian, the contents of tetrandrine, palmatine and epiberberine are extremely low, and the content of jatrorrhizine is relatively high. The specific results are shown in Table 4.

表4各药材中各生物碱含量Each alkaloid content in each medical material of table 4

黄连品种不同,色度及生物碱含量不同。云连及日本黄连a*值少,而且非洲防己碱、巴马汀,表小檗碱含量极端少。对味连中a*值与小檗碱含量有相关性(C光2°视场:R2=0.72,F10光10°视场:R2=0.75)具体见图2所示。研究还发现,同一产地同一品种同一采集时间,1級品黄连比2級品或3級品色度(L*、a*及b*)高、同時总生物碱含量高。不同等級的药材是药材大小不同、是色度不同、是生物碱含量有差异。Different varieties of Coptis chinensis have different chroma and alkaloid content. The a* value of Yunlian and Coptis chinensis is low, and the contents of tetrandrine, palmatine and epiberberine are extremely low. There is a correlation between a* value and berberine content in Milian (C light 2° field of view: R 2 =0.72, F10 light 10° field of view: R 2 =0.75). See Figure 2 for details. The study also found that, in the same place of origin, the same variety, and the same collection time, the first-grade Coptidis rhizome had higher color (L*, a* and b*) and higher total alkaloid content than the second-grade or third-grade varieties. Different grades of medicinal materials are different in size, color, and alkaloid content.

Claims (1)

1. a Rhizoma Coptidis colourity digitlization quality detecting method, is characterized in that: comprise the following steps:
1) Rhizoma Coptidis is pulverized, obtained Golden Thread;
2) Golden Thread is placed in to cuvette, adopts photoelectric tristimulus colorimetry or color measurement by spectrophotometry to determine tristimulus values X, Y, Z;
3) tristimulus values X, Y, Z are calculated and provide L*,a*,b*
4) pass through L*,a*,b*Kind and the quality of the position judgment Rhizoma Coptidis in coordinate system;
Step 4) is by reading L*,a*,b*Value, judge coptis chinensis total alkaloid content;
Step 4) is by judging a*,b*The lane place in coordinate system between, judge the kind of the coptis;
Described checkout equipment comprises colour photometer, light source and cuvette; Wherein cuvette is placed in thermostat; Described light source is markAccurate A light, C light, D65 light, D50 light, ID65 light, ID50 light, F2, F6, F7, F8, F10 light, F11, a kind of light source in F12, shinesBright mode is diffused illumination, reverberation; The field of view angle of described colour photometer is 2 ° and 10 °.
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