鹿角胶

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

概述 Overview

本品为鹿角经水煎煮、浓缩制成的固体胶。
Deer Horn Glue is the solid glue made by decocting and concentrating deer horn.

制法 Processing

将鹿角锯段，漂泡洗净，分次水煎，滤过，合并滤液（或加入白矾细粉少量），静置，滤取胶液，浓缩（可加适量黄酒、冰糖和豆油）至稠膏状，冷凝，切块，晾干，即得。
Cut deer horn into sections, wash and soak, decoct in water in several portions, filter, combine the filtrate (or add a small amount of alum powder), let it stand, filter the glue liquid, concentrate (may add appropriate amount of yellow rice wine, rock sugar, and soybean oil) to a thick paste, condense, cut into pieces, and dry to obtain the product.

性状 Description

本品呈扁方形块或丁状。黄棕色或红棕色，半透明，有的上部有黄白色泡沫层。质脆，易碎，断面光亮。气微，味微甜。
It is flat square or cuboid. Yellowish-brown or reddish-brown, semi-transparent, some with yellowish-white foam on the surface. Brittle, easily broken, with a shiny fracture. Slight odor, slightly sweet taste.

鉴别 Identification

取本品粉末0.1 g，加1%碳酸氢铵溶液50 ml，超声处理30分钟，用微孔滤膜滤过，取续滤液100 μl，置微量进样瓶中，加胰蛋白酶溶液10 μl（取序列分析用胰蛋白酶，加1%碳酸氢铵溶液制成每1 ml中含1 mg的溶液，临用时配制），摇匀，37 ℃恒温酶解12小时，作为供试品溶液。另取鹿角胶对照药材0.1 g，同法制成对照药材溶液。照高效液相色谱法-质谱法（通则0512和通则0431）试验，以十八烷基硅烷键合硅胶为填充剂（色谱柱内径2.1 mm）；以乙腈为流动相A，以0.1%甲酸溶液为流动相B，按下表中的规定进行梯度洗脱；流速为每分钟0.3 ml。采用质谱检测器，电喷雾正离子模式（ESI+），进行多反应监测（MRM），选择质荷比（m/z）765.4（双电荷）→554.0和m/z765.4（双电荷）→733.0作为检测离子对。取鹿角胶对照药材溶液，进样5 μl，按上述检测离子对测定的MRM色谱峰的信噪比均应大于3︰1。
To 0.1 g of the powder add 50 ml of 1% ammonium bicarbonate solution, treat with ultrasound for 30 minutes, filter through a microporous membrane, take 100 μl of the filtrate, place it in a microsampling bottle, add 10 μl of trypsin solution (take trypsin for sequence analysis, prepare a solution containing 1 mg per ml with 1% ammonium bicarbonate solution before use), shake well, and incubate at 37°C for 12 hours as the test solution. Take 0.1 g of the reference drug deer horn glue and prepare the reference drug solution by the same method. Perform the test according to the high-performance liquid chromatography-mass spectrometry method (General Rule 0512 and General Rule 0431), using octadecylsilane-bonded silica gel as the filling material (column inner diameter 2.1 mm); use acetonitrile as mobile phase A and 0.1% formic acid solution as mobile phase B, and perform gradient elution according to the specified conditions in the table; the flow rate is 0.3 ml per minute. Use a mass spectrometry detector, electrospray ionization positive ion mode (ESI+), and perform multiple reaction monitoring (MRM), selecting the mass-to-charge ratio (m/z) 765.4 (double charge)→554.0 and m/z 765.4 (double charge)→733.0 as the detection ion pairs. Inject 5 μl of the deer horn glue reference drug solution, and the signal-to-noise ratio of the MRM chromatographic peak determined by the above detection ion pairs should be greater than 3:1.

吸取供试品溶液5 μl，注入高效液相色谱-质谱联用仪，测定。以质荷比（m/z）765.4（双电荷）→554.0和m/z765.4（双电荷）→733.0离子对提取的供试品离子流色谱中，应同时呈现与对照药材色谱保留时间一致的色谱峰。
Take 5 μl of the test solution, inject it into the high-performance liquid chromatography-mass spectrometry system, and determine it. In the ion flow chromatogram extracted by the mass-to-charge ratio (m/z) 765.4 (double charge)→554.0 and m/z 765.4 (double charge)→733.0 ion pairs, a chromatographic peak that is consistent with the retention time of the reference drug should be simultaneously present.

检查 Examination

水分 Water

取本品1 g，精密称定，加水2 ml，加热溶解后，置水浴上蒸干，使厚度不超过2 mm，照水分测定法（通则0832第二法）测定，不得过15.0%。
Weigh accurately 1 g of the product, add 2 ml of water, dissolve by heating, place it on a water bath and evaporate until the thickness does not exceed 2 mm, and determine the water content according to the method for water determination (General Rule 0832, method 2), which should not exceed 15.0%.

总灰分 Total ash

取本品1.0 g，依法检查（通则2302），不得过3.0%。
Take 1.0 g of the product and examine it according to the regulations (General Rule 2302), which should not exceed 3.0%.

重金属 Heavy metals

取总灰分项下的残渣，依法检查（通则0821第二法），不得过30 mg/kg。
Take the residue under the total ash item and examine it according to the regulations (General Rule 0821, method 2), which should not exceed 30 mg/kg.

砷盐 Arsenic salts

取本品1.0 g，加氢氧化钙1 g，混合，加少量水，搅匀，干燥后，先用小火烧灼使炭化，再在500～600 ℃炽灼使完全灰化，放冷，加盐酸5 ml与水2 ml，依法检查（通则0822），不得过2 mg/kg。
Take 1.0 g of the product, add 1 g of calcium hydroxide, mix, add a small amount of water, stir well, dry, first carbonize with low heat, then incinerate at 500-600°C to complete ashing, cool, add 5 ml of hydrochloric acid and 2 ml of water, and examine it according to the regulations (General Rule 0822), which should not exceed 2 mg/kg.

水中不溶物 Insoluble matter in water

取本品1.0 g，精密称定，加水10 ml，加热溶解，将溶液移入已恒重的10 ml离心管中，离心，去除管壁浮油，倾去上清液，沿管壁加入温水至刻度，离心，如法清洗3次，倾去上清液，离心管在105 ℃加热2小时，取出，置干燥器中冷却30分钟，精密称定，计算，即得。
Weigh accurately 1.0 g of the product, add 10 ml of water, dissolve by heating, transfer the solution to a 10 ml centrifuge tube that has been weighed, centrifuge, remove the oil floating on the tube wall, pour off the supernatant, add warm water along the tube wall to the mark, centrifuge, wash 3 times as before, pour off the supernatant, heat the centrifuge tube at 105°C for 2 hours, take it out, cool it in a desiccator for 30 minutes, weigh accurately, and calculate to obtain the result.

本品水中不溶物不得过2.0%。
The insoluble matter in water of the product should not exceed 2.0%.

其他 Others

应符合胶剂项下有关的各项规定（通则0184）。
It should comply with the relevant regulations under the adhesive item (General Rule 0184).

含量测定 Assay

照高效液相色谱法（通则0512）测定。
Determine by high-performance liquid chromatography (General Rule 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；以乙腈-0.1 mol/L醋酸钠溶液（用醋酸调节pH值至6.5）（7︰93）为流动相A，以乙腈-水（4︰1）为流动相B，按下表中的规定进行梯度洗脱；检测波长为254 nm。柱温为43 ℃。理论板数按L-羟脯氨酸峰计算应不低于4000。
Use octadecylsilane-bonded silica gel as the filling material; use acetonitrile-0.1 mol/L sodium acetate solution (adjust the pH value to 6.5 with acetic acid) (7:93) as mobile phase A, and use acetonitrile-water (4:1) as mobile phase B. Perform gradient elution according to the specified conditions in the table; the detection wavelength is 254 nm. The column temperature is 43°C. The theoretical plate number calculated based on the peak of L-hydroxyproline should not be less than 4000.

对照品溶液的制备 Preparation of reference solution

取L-羟脯氨酸对照品、甘氨酸对照品、丙氨酸对照品、L-脯氨酸对照品适量，精密称定，加0.1 mol/L盐酸溶液制成每1 ml含L-羟脯氨酸70 μg、甘氨酸0.14 mg、丙氨酸60 μg 、L-脯氨酸70 μg的混合溶液，即得。
Take an appropriate amount of L-hydroxyproline reference substance, glycine reference substance, alanine reference substance, and L-proline reference substance, weigh accurately, and add 0.1 mol/L hydrochloric acid solution to prepare a mixed solution containing 70 μg of L-hydroxyproline, 0.14 mg of glycine, 60 μg of alanine, and 70 μg of L-proline per 1ml.

供试品溶液的制备 Preparation of test solution

取本品粗粉约0.25 g，精密称定，置25 ml量瓶中,加0.1 mol/L盐酸溶液20 ml，超声处理（功率300 W，频率40 kHz）30分钟，放冷，加0.1 mol/L盐酸溶液至刻度，摇匀。精密量取2 ml，置5 ml安瓿中，加盐酸2 ml，150 ℃水解1小时，放冷，移至蒸发皿中，用水10 ml分次洗涤，洗液并入蒸发皿中，蒸干，残渣加0.1 mol/L盐酸溶液溶解，转移至25 ml量瓶中，加0.1 mol/L盐酸溶液至刻度，摇匀，即得。
Take about 0.25 g of the crude powder of the product, weigh accurately, place it in a 25 ml volumetric flask, add 20 ml of 0.1 mol/L hydrochloric acid solution, treat with ultrasound (power 300 W, frequency 40 kHz) for 30 minutes, cool, add 0.1 mol/L hydrochloric acid solution to the mark, shake well. Accurately measure 2 ml, place it in a 5 ml ampoule, add 2ml of hydrochloric acid, hydrolyze at 150°C for 1 hour, cool, transfer to an evaporating dish, wash with water in portions of 10 ml, pour the washing liquid into the evaporating dish, evaporate to dryness, dissolve the residue in 0.1 mol/L hydrochloric acid solution, transfer to a 25 ml volumetric flask, add 0.1 mol/L hydrochloric acid solution to the mark, shake well.

精密量取上述对照品溶液和供试品溶液各5 ml，分别置25 ml量瓶中，各加0.1 mol/L异硫氰酸苯酯（PITC）的乙腈溶液2.5 ml，1 mol/L三乙胺的乙腈溶液2.5 ml，摇匀，室温放置1小时后，加50%乙腈至刻度，摇匀。取10 ml，加正己烷10 ml，振摇，放置10分钟，取下层溶液，滤过，取续滤液，即得。
Accurately measure 5 ml of the above reference solution and test solution, place them in separate 25 ml volumetric flasks, add 2.5 ml of acetonitrile solution of 0.1 mol/L phenyl isothiocyanate (PITC) and 2.5 ml of acetonitrile solution of 1 mol/L triethylamine, shake well, and let it stand at room temperature for 1 hour. Add 50% acetonitrile to the mark, shake well. Take 10 ml, add 10 ml of n-hexane, shake, let it stand for 10 minutes, take the lower layer solution, filter, and take the subsequent filtrate.

测定法 Assay method

分别精密吸取衍生化后的对照品溶液与供试品溶液各5 μl，注入液相色谱仪，测定，即得。
Accurately suck 5 μl of the derivatized reference solution and test solution, inject them into the liquid chromatograph, and determine.

本品按干燥品计算，含L-羟脯氨酸不得少于6.6%、甘氨酸不得少于13.3%、丙氨酸不得少于5.2%、L-脯氨酸不得少于7.5%。
Calculated on the basis of the dried product, the content of L-hydroxyproline should not be less than 6.6%, glycine should not be less than 13.3%, alanine should not be less than 5.2%, and L-proline should not be less than 7.5%.

性 Property

温。
Warm.

味 Flavor

甘、咸。
Sweet and salty.

归经 Meridian tropism

归肾、肝经。
Kidney and liver meridians.

功能 Actions

温补肝肾，益精养血。
It warms and tonifies the liver and kidney, nourishes essence and blood.

主治 Indications

用于肝肾不足所致的腰膝酸冷，阳痿遗精，虚劳羸瘦，崩漏下血，便血尿血，阴疽肿痛。
It is used for lumbago and coldness of the waist and knees caused by liver and kidney deficiency, impotence and premature ejaculation, weakness and emaciation, excessive uterine bleeding, bloody stools, bloody urine, and swelling and pain of carbuncle.

用量 Dosage

3～6 g。
3-6 g.

用法 Administration

烊化兑服。
Decocted and taken orally.

规格 Specification

每块重6g。
Each piece weighs 6g.

贮藏 Storage

密闭。
Store in a sealed container.