王不留行

中文文本参考：《中国药典（2020年版）》
English text reference: Chinese Pharmacopoeia (2020 Edition)

概述 Overview

本品为石竹科植物麦蓝菜Vaccaria segetalis（Neck.）Garcke的干燥成熟种子。夏季果实成熟、果皮尚未开裂时采割植株，晒干，打下种子，除去杂质，再晒干。
Vaccaria Seed is the dried mature seed of Vaccaria segetalis (Neck.) Garcke (Fam. Caryophyllaceae). The drug is collected in summer when the fruit is ripe but the pericarp has not yet split, removed from foreign matter, and dried in the sun.

性状 Description

本品呈球形，直径约2 mm。表面黑色，少数红棕色，略有光泽，有细密颗粒状突起，一侧有1凹陷的纵沟。质硬。胚乳白色，胚弯曲成环，子叶2。气微，味微涩、苦。
Seeds spherical, about 2 mm in diameter. Surface black, a few reddish-brown, slightly shiny, with fine granular projections, one side with a longitudinal groove. Texture hard. Endosperm white, embryo curved into a ring, cotyledons 2. Odour, slight; taste, slightly astringent and bitter.

鉴别 Identification

（1）本品粉末淡灰褐色。种皮表皮细胞红棕色或黄棕色，表面观多角形或长多角形，直径50～120 μm，垂周壁增厚，星角状或深波状弯曲。种皮内表皮细胞淡黄棕色，表面观类方形、类长方形或多角形，垂周壁呈紧密的连珠状增厚，表面可见网状增厚纹理。胚乳细胞多角形、类方形或类长方形，胞腔内充满淀粉粒和糊粉粒。子叶细胞含有脂肪油滴。
(1) The powder is pale grayish-brown. Epidermal cells of the testa reddish-brown or yellowish-brown, viewed from the surface polygonal or elongated polygonal, 50-120 μm in diameter, with thickened walls on the tangential side, star-shaped or deeply undulate. Subepidermal cells of the testa pale yellowish-brown, viewed from the surface square or elongated square or polygonal, with closely arranged tangential walls, surface with reticulate thickening. Endosperm cells polygonal, square or elongated square, filled with starch granules and protein granules in the cell cavity. Cotyledon cells contain oil droplets.

（2）取本品粉末1.5 g，加甲醇20 ml，加热回流30分钟，放冷，滤过，滤液回收溶剂至干，残渣加甲醇2 ml使溶解，作为供试品溶液。另取王不留行对照药材1.5 g，同法制成对照药材溶液。再取王不留行黄酮苷对照品和刺桐碱对照品，加甲醇制成每1 ml分别含0.2 mg和1 mg的溶液，作为对照品溶液。照薄层色谱法（通则0502）试验，吸取上述四种溶液各5 μl，分别点于同一硅胶G薄层板上，以三氯甲烷-甲醇-水（15∶7∶2）的下层溶液为展开剂，展开，取出，晾干，喷以2%三氯化铝乙醇溶液，热风吹干，置紫外光灯（365 nm）下检视。供试品色谱中，在与对照药材色谱和王不留行黄酮苷对照品色谱相应的位置上，显相同颜色的荧光斑点。再置碘蒸气中熏至斑点显色清晰，置日光下检视。供试品色谱中，在与对照药材色谱和刺桐碱对照品色谱相应的位置上，显相同颜色的斑点。
(2) To 1.5 g of the powder add 20 ml of methanol, heat under reflux for 30 minutes, cool, filter, evaporate the filtrate to dryness, dissolve the residue in 2 ml of methanol as the test solution. Take 1.5 g of the reference drug of Vaccaria Seed, prepare the reference drug solution by the same method. Take the reference substances of Vaccaria Seed Flavonoids and Vaccarin, dissolve them in methanol to produce solutions containing 0.2 mg and 1 mg per ml, respectively, as the reference solution. Carry out the method for thin layer chromatography<0502>, using silica gel G as the coating substance and a mixture of chloroform-methanol-water (15:7:2) as the lower layer of the mobile phase. Apply separately to the plate 5 μl of each of the above four solutions. After developing and removal of the plate, dry in air. Spray with a 2% solution of aluminum chloride in ethanol, dry with hot air, examine under ultraviolet light at 365 nm. The fluorescent spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the reference drug solution and the spot in the chromatogram obtained with the reference solution of Vaccaria Seed Flavonoids. Expose to iodine vapour until the spots appear clearly, examine under daylight. The spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the reference drug solution and the spot in the chromatogram obtained with the reference solution of Vaccarin.

检查 Examination

水分 Water

不得过12.0%（通则0832第二法）。
Not more than 12.0 per cent <0832,method 2>.

总灰分 Total ash

不得过4.0%（通则2302）。
Not more than 4.0 per cent <2302>.

浸出物 Extractives

照醇溶性浸出物测定法（通则2201）项下的热浸法测定，用乙醇作溶剂，不得少于6.0%。
Carry out the method for determination of ethanol-soluble Extractives <2201,the hot maceration method>, using ethanol as the solvent,not less than 6.0 per cent.

含量测定 Content determination

照高效液相色谱法（通则0512）测定。
Carry out the method for determination of content by high performance liquid chromatography <0512>.

色谱条件与系统适用性试验 Chromatographic conditions and system suitability test

以十八烷基硅烷键合硅胶为填充剂；以甲醇为流动相A，以0.3%磷酸溶液为流动相B，按下表中的规定进行梯度洗脱；检测波长为280 nm。理论板数按王不留行黄酮苷峰计算应不低于3000。
Use octadecylsilane bonded silica gel as the filler; use methanol as mobile phase A, and 0.3% phosphoric acid solution as mobile phase B. Perform gradient elution according to the specified conditions in the table; detect at a wavelength of 280nm. The theoretical plate number calculated based on the peak of baicalin should not be less than 3000.

对照品溶液的制备 Preparation of reference solution

取王不留行黄酮苷对照品适量，精密称定，加70%甲醇制成每1 ml含0.1 mg的溶液，即得。
Take an appropriate amount of baicalin reference substance, accurately weigh, add 70% methanol to make a solution containing 0.1 mg per 1 ml.

供试品溶液的制备 Preparation of test solution

取本品粉末（过三号筛）约1.2 g，精密称定，置具塞锥形瓶中，精密加入70%甲醇50 ml，称定重量，超声处理（功率250 W，频率33 kHz）30分钟，放冷，再称定重量，用70%甲醇补足减失的重量，摇匀，滤过，取续滤液，即得。
Take about 1.2 g of the powder of this medicinal material (passed through a No. 3 sieve), accurately weigh, place it in a stoppered conical flask, accurately add 50 ml of 70% methanol, weigh, subject to ultrasonic treatment (power 250 W, frequency 33 kHz) for 30 minutes, cool, weigh again, make up the weight lost with 70% methanol, shake well, filter, and take the filtrate to obtain the test solution.

测定法 Determination method

分别精密吸取对照品溶液与供试品溶液各10 μl，注入液相色谱仪，测定，即得。
Accurately aspirate 10 μl of the reference solution and the test solution respectively, inject into the liquid chromatograph, and determine to obtain the results.

本品按干燥品计算，含王不留行黄酮苷（C32H38O19）不得少于0.40%。
Calculated on the dried product, the content of baicalin (C32H38O19) should not be less than 0.40%.

饮片 Prepared slices

王不留行 Baical Skullcap Root

炮制 Processing

除去杂质。
Eliminate Foreign matter.

性状 Characteristics

同药材。
Same as the crude drug.

鉴别 Identification

同药材。
Same as the crude drug.

检查 Examination

同药材。
Same as the crude drug.

浸出物 Extractives

同药材。
Same as the crude drug.

含量测定 Content determination

同药材。
Same as the crude drug.

炒王不留行 Stir-fried Baical Skullcap Root

炮制 Processing

取净王不留行，照清炒法（通则0213）炒至大多数爆开白花。
Take clean Baical Skullcap Root, stir-fry according to the method of stir-frying until most of them burst into white flowers.

性状 Characteristics

本品呈类球形爆花状，表面白色，质松脆。
This product is spherical with burst flowers, white surface, and loose and crisp texture.

检查 Examination

水分 Water

同药材，不得过10.0%。
Water Same as the crude drug, not more than 10.0 per cent.

含量测定 Content determination

同药材，含王不留行黄酮苷（C32H38O19）不得少于0.15%。
Same as the crude drug, the content of baicalin (C32H38O19) should not be less than 0.15%.

鉴别 Identification

（除显微粉末外）同药材。
(Except for microscopic powder) Same as the crude drug.

浸出物 Extractives

同药材。
Same as the crude drug.

性 Property

平。
Neutral.

味 Flavor

苦。
Bitter.

归经 Meridian tropism

归肝、胃经。
Liver and stomach meridians.

功能 Actions

活血通经，下乳消肿，利尿通淋。
Promote blood circulation and regulate menstruation, reduce swelling and promote lactation, diuretic and relieve stranguria.

主治 Indications

用于经闭，痛经，乳汁不下，乳痈肿痛，淋证涩痛。
Used for amenorrhea, dysmenorrhea, insufficient lactation, breast abscess with swelling and pain, stranguria with pain.

用量 Dosage

5～10 g。
5-10 g.

用法 Administration

无。
None.

注意 Precautions

孕妇慎用。
Use with caution in pregnant women.

贮藏 Storage

置干燥处。
Store in a dry place.

王不留行

文本参考：《中国药典（2015年版）》
Text reference: Chinese Pharmacopoeia (2015 Edition)

概述 Overview

本品为石竹科植物麦蓝菜Vaccaria segetalis（Neck.）Garcke的干燥成熟种子。夏季果实成熟、果皮尚未开裂时采割植株，晒干，打下种子，除去杂质，再晒干。
Cowherb Seed is the dried ripe seed of Vaccaria segetalis (Neck.) Garcke (Fam. Caryophyllaceae). The plant is collected in summer when the fruit is ripe but not dehiscent, and dried in the sun, the seed is tapped out, removed from foreign matter, and dried again in the sun.

性状 Description

本品呈球形，直径约2mm。表面黑色，少数红棕色，略有光泽，有细密颗粒状突起，一侧有1凹陷的纵沟。质硬。胚乳白色，胚弯曲成环，子叶2。气微，味微涩、苦。
Spheroidal, about 2 mm in diameter. Externally black, a few in reddish-brown, somewhat lustrous, with fine and dense granular protuberances and a concave longitudinal furrow on one side. Texture hard, endosperm white, embryo curved in a ring, cotyledons 2. Odour, slight; taste, slightly astringent and bitter.

鉴别 Identification

（1）本品粉末淡灰褐色。种皮表皮细胞红棕色或黄棕色，表面观多角形或长多角形，直径50～120μm，垂周壁增厚，星角状或深波状弯曲。种皮内表皮细胞淡黄棕色，表面观类方形、类长方形或多角形，垂周壁呈紧密的连珠状增厚，表面可见网状增厚纹理。胚乳细胞多角形、类方形或类长方形，胞腔内充满淀粉粒和糊粉粒。子叶细胞含有脂肪油滴。
（2）取本品粉末1.5g，加甲醇20ml，加热回流30分钟，放冷，滤过，滤液蒸干，残渣加甲醇2ml使溶解，作为供试品溶液。另取王不留行对照药材1.5g，同法制成对照药材溶液。照薄层色谱法（通则0502）试验，吸取上述两种溶液各10μl，分别点于同一硅胶G薄层板上，以三氯甲烷-甲醇-水（15：7：2）的下层溶液为展开剂，展开，取出，晾干，喷以改良碘化铋钾试液。供试品色谱中，在与对照药材色谱相应的位置上，显相同的橙红色斑点。

检查 Examination

水分 Water

不得过12.0%（通则0832第二法）。
Not more than 12.0 per cent <0832, method 2>.

总灰分 Total ash

不得过4.0%（通则2302）。
Not more than 4.0 per cent <2302>.

浸出物 Extractives

照醇溶性浸出物测定法（通则2201）项下的热浸法测定，用乙醇作溶剂，不得少于6.0%。
Carry out the hot extraction method for determination of ethanol-soluble extractives <2201>, using ethanol as the solvent, not less than 6.0 per cent.

含量测定 Assay

照高效液相色谱法（通则0512）测定。
Carry out the method for high performance liquid chromatography <0512>.

色谱条件与系统适用性试验 Chromatographic system and system suitability

以十八烷基硅烷键合硅胶为填充剂；以甲醇为流动相A，以0.3%磷酸溶液为流动相B，按下表中的规定进行梯度洗脱；检测波长为280nm。理论板数按王不留行黄酮苷峰计算应不低于3000。

时间（分钟） 流动相A（%） 流动相B（%）

0～10
35
65
10～20
35→40
65→60
20～35
40→50
60→50

对照品溶液的制备
取王不留行黄酮苷对照品适量，精密称定，加70%甲醇制成每1ml含0.1mg的溶液，即得。