制川乌

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

概述 Overview

本品为川乌的炮制加工品。
Processed Aconite Root is the processed product of Aconitum carmichaeli Debx. (Fam. Ranunculaceae).

炮制 Processing

取川乌，大小个分开，用水浸泡至内无干心，取出，加水煮沸4～6小时（或蒸6～8小时）至取大个及实心者切开内无白心，口尝微有麻舌感时，取出，晾至六成干，切片，干燥。
Take Aconite Root, separate the large and small ones, soak in water until there is no dry heart inside, remove, boil in water for 4-6 hours (or steam for 6-8 hours) until the large and solid ones are cut open and there is no white heart inside, remove, dry until 60% dry, slice, and dry.

性状 Description

本品为不规则或长三角形的片。表面黑褐色或黄褐色，有灰棕色形成层环纹。体轻，质脆，断面有光泽。气微，微有麻舌感。
Irregular or long triangular pieces; surface blackish-brown or yellowish-brown, with greyish-brown formed layer ringed. Light in weight, brittle in texture, and glossy on the fracture surface. Odour, slight; taste, slightly tingling on the tongue.

鉴别 Identification

取本品粉末2g，加氨试液2ml润湿，加乙醚20ml，超声处理30分钟，滤过，滤液挥干，残渣加二氯甲烷1ml使溶解，作为供试品溶液。另取苯甲酰乌头原碱对照品、苯甲酰次乌头原碱对照品及苯甲酰新乌头原碱对照品，加异丙醇-三氯甲烷（1∶1）混合溶液制成每1ml各含1mg的混合溶液，作为对照品溶液。照薄层色谱法（通则0502）试验，吸取上述两种溶液各5μl，分别点于同一硅胶G薄层板上，以正己烷-乙酸乙酯-甲醇（6.4∶3.6∶1）为展开剂，置氨蒸气饱和20分钟的展开缸内，展开，取出，晾干，喷以稀碘化铋钾试液。供试品色谱中，在与对照品色谱相应的位置上，显相同颜色的斑点。
To 2g of the powder add 2ml of ammonia TS, moisten, add 20ml of ether, treat with ultrasound for 30 minutes, filter, evaporate the filtrate to dryness, dissolve the residue in 1ml of methylene chloride as the test solution. Take aconitine CRS, benzoylaconine CRS, and benzoylhypaconine CRS, dissolve each in a mixture of isopropanol and chloroform (1:1) to produce a solution containing 1mg per ml 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 n-hexane, glacial acetic acid, and methanol (6.4:3.6:1) as the mobile phase. Place the plate in a developing cylinder saturated with ammonia vapour for 20 minutes, develop, remove, dry in air, and spray with a solution of iodine in potassium iodide TS. 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 solution.

检查 Examination

水分 Water

不得过11.0%（通则0832第二法）。
Not more than 11.0 per cent <0832,method 2>.

双酯型生物碱 Bisbenzylisoquinoline alkaloids

照〔含量测定〕项下色谱条件、供试品溶液的制备方法试验。
Follow the test method for preparation of the sample solution and chromatographic conditions under the determination of content.

对照品溶液的制备 Preparation of reference solution

取乌头碱对照品、次乌头碱对照品及新乌头碱对照品适量，精密称定，加异丙醇-三氯甲烷（1∶1）混合溶液分别制成每1ml含乌头碱50μg、次乌头碱和新乌头碱各0.15mg的混合溶液，即得。
Take appropriate amounts of aconitine reference standard, mesaconitine reference standard, and hypaconitine reference standard, accurately weigh, add a mixture of isopropanol and chloroform (1:1) to prepare a mixed solution containing 50μg of aconitine and 0.15mg each of mesaconitine and hypaconitine in 1ml.

测定法 Determination method

分别精密吸取对照品溶液与〔含量测定〕项下供试品溶液各10μl，注入液相色谱仪，测定，即得。
Accurately aspirate 10μl of the reference solution and the sample solution under the determination of content, inject into the liquid chromatograph, and determine.

本品含双酯型生物碱以乌头碱（C34H47NO11）、次乌头碱（C33H45NO10）及新乌头碱（C33H45NO11）的总量计，不得过0.040%。
This product contains diester alkaloids, calculated by the total amount of aconitine (C34H47NO11), hypoaconitine (C33H45NO10) and neoaconitine (C33H45NO11), not more than 0.040%.

含量测定 Content determination

照高效液相色谱法（通则0512）测定。
Determine according to the high performance liquid chromatography method <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-四氢呋喃（25∶15）为流动相A，以0.1mol/L醋酸铵溶液（每1000ml加冰醋酸0.5ml）为流动相B，按下表中的规定进行梯度洗脱；检测波长为235nm。理论板数按苯甲酰新乌头原碱峰计算应不低于2000。
Use octadecylsilane bonded silica gel as the filler; use acetonitrile-tetrahydrofuran (25:15) as mobile phase A, and 0.1mol/L ammonium acetate solution (add 0.5ml of glacial acetic acid to each 1000ml) as mobile phase B. Perform gradient elution according to the specified conditions in the table; the detection wavelength is 235nm. The theoretical plate number calculated based on the peak of benzoylhypaconine should not be less than 2000.

对照品溶液的制备 Preparation of reference solution

取苯甲酰乌头原碱对照品、苯甲酰次乌头原碱对照品、苯甲酰新乌头原碱对照品适量，精密称定，加异丙醇-三氯甲烷（1∶1）混合溶液制成每1ml含苯甲酰乌头原碱和苯甲酰次乌头原碱各50μg、苯甲酰新乌头原碱0.3mg的混合溶液，即得。
Take appropriate amounts of benzoylaconine reference standard, benzoylmesaconine reference standard, and benzoylhypaconine reference standard, accurately weigh, and add a mixture of isopropanol and chloroform (1:1) to prepare a mixed solution containing 50μg each of benzoylaconine and benzoylmesaconine and 0.3mg of benzoylhypaconine in 1ml.

供试品溶液的制备 Preparation of sample solution

取本品粉末（过三号筛）约2g，精密称定，置具塞锥形瓶中，加氨试液3ml，精密加入异丙醇-乙酸乙酯（1∶1）混合溶液50ml，称定重量，超声处理（功率300W，频率40kHz；水温在25℃以下）30分钟，放冷，再称定重量，用异丙醇-乙酸乙酯（1：1）混合溶液补足减失的重量，摇匀，滤过。精密量取续滤液25ml，40℃以下减压回收溶剂至干，残渣精密加入异丙醇-三氯甲烷（1∶1）混合溶液3ml溶解，滤过，取续滤液，即得。
Take about 2g of this product powder (passed through a No. 3 sieve), accurately weigh, place it in a stoppered conical flask, add 3ml of ammonia test solution, accurately add a mixture of isopropanol and ethyl acetate (1:1) 50ml, weigh, treat with ultrasound (power 300W, frequency 40kHz; water temperature below 25℃) for 30 minutes, cool, weigh again, make up for the lost weight with a mixture of isopropanol and ethyl acetate (1:1), shake well, and filter. Accurately take 25ml of the filtrate, reduce the pressure below 40℃ to recover the solvent to dryness, accurately add 3ml of a mixture of isopropanol and chloroform (1:1) to dissolve the residue, filter, and take the filtrate.

测定法 Determination method

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

本品按干燥品计算，含苯甲酰乌头原碱（C32H45NO10）、苯甲酰次乌头原碱（C31H43NO9）及苯甲酰新乌头原碱（C31H43NO10）的总量应为0.070%～0.15%。
Calculated on the dried product, the total amount of benzoylaconine (C32H45NO10), benzoylmesaconine (C31H43NO9), and benzoylhypaconine (C31H43NO10) in this product should be 0.070% to 0.15%.

性 Property

热。
Hot.

味 Flavor

辛，苦。
Pungent and bitter.

归经 Meridian tropism

归心、肝、肾、脾经。
Heart, Liver, Kidney, Spleen meridians.

功能 Actions

祛风除湿，温经止痛。
Expel wind and eliminate dampness, warm the meridians and relieve pain.

主治 Indications

用于风寒湿痹，关节疼痛，心腹冷痛，寒疝作痛及麻醉止痛。
Used for wind-cold-damp arthralgia, joint pain, cold pain in the abdomen, cold hernia pain, and anesthesia analgesia.

用量 Dosage

1.5～3g。
1.5-3g.

用法 Administration

先煎、久煎。
Decoct first, and decoct for a long time.

注意 Precautions

孕妇慎用；不宜与半夏、瓜蒌、瓜蒌子、瓜蒌皮、天花粉、川贝母、浙贝母、平贝母、伊贝母、湖北贝母、白蔹、白及同用。
Caution for pregnant women; avoid using with pinellia, trichosanthes root, trichosanthes seed, trichosanthes peel, datura pollen, fritillaria cirrhosa, fritillaria thunbergii, fritillaria pallidiflora, fritillaria verticillata, fritillaria hupehensis, arisaema, and atractylodes.

贮藏 Storage

置通风干燥处，防蛀。
Store in a well-ventilated and dry place, and protect against moth.

制川乌

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

概述 Overview

本品为川乌的炮制加工品。
The drug is the processed Aconiti Radix.

制法 Processing

取川乌，大小个分开，用水浸泡至内无干心，取出，加水煮沸4～6小时（或蒸6～8小时）至取大个及实心者切开内无白心，口尝微有麻舌感时，取出，晾至六成干，切片，干燥。
Processing Grade clean Aconiti Radix according to size, macerate in water until there is no dry core. Take out, boil in water for 4 to 6 hours (or steam for 6 to 8 hours) until there is no white core in the relatively large and solid root and the taste becomes slightly numb. Take out, dry in the air appropriately, cut into slices, and dry.

性状 Description

本品为不规则或长三角形的片。表面黑褐色或黄褐色，有灰棕色形成层环纹。体轻，质脆，断面有光泽。气微，微有麻舌感。
Irregular or elongated triangular slices. Externally dark brown or yellowish-brown, with a greyish-brown cambium ring, Texture light and fragile, fracture lustrous. Odour, slight； taste, slightly numb.

鉴别 Identification

取本品粉末2g，加氨试液2ml润湿，加乙醚20ml，超声处理30分钟，滤过，滤液挥干，残渣加二氯甲烷1ml使溶解，作为供试品溶液。另取苯甲酰乌头原碱对照品、苯甲酰次乌头原碱对照品及苯甲酰新乌头原碱对照品，加异丙醇-三氯甲烷（1：1）混合溶液制成每1ml各含1mg的混合溶液，作为对照品溶液。照薄层色谱法（通则0502）试验，吸取上述两种溶液各5μl分别点于同一硅胶G薄层板上，以正己烷-乙酸乙酯-甲醇（6.4：3.6：1）为展开剂，置氨蒸气饱和20分钟的展开缸内，展开，取出，晾干，喷以稀碘化铋钾试液。供试品色谱中，在与对照品色谱相应的位置上，显相同颜色的斑点。
Moisten 2 g of the powder with 2 ml of ammonia concentrated TS, add 20 ml of ether, ultrasonicate for 30 minutes and filter. Evaporate the filtrate to dryness, dissolve the residue in 1 ml of dichloromethane as the test solution. Dissolve benzoylaconine CRS, benzoylhypaconitine CRS and benzoylmesaconitine CRS in a mixture of isopropanol and chloroform (1 : 1) to produce a mixture containing 1 mg of each per ml 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 n-hexane, ethyl acetate and methanol (6.4 : 3.6 : 1) as the mobile phase. Apply separately 5 μl of each of the above two solutions to the plate. After developing in a chamber pre-equilibrated with the vapour of ammonia for 20 minutes, removal of the plate, dry in air. Spray with dilute potassium iodobismuthate TS. The spots in the chromatogram obtained with the test solution correspond in position and colour to the spots in the chromatogram obtained with the reference solution.

检查 Examination

水分 Water

不得过11.0%（通则0832第二法）。
Not more than 11.0 per cent <0832, method 2>.

双酯型生物碱 Diester-alkaloids

照〔含量测定〕项下色谱条件、供试品溶液的制备方法试验。
Carry out the method for high performance liquid chromatography<0512>.

对照品溶液的制备 Reference solution

取乌头碱对照品、次乌头碱对照品及新乌头碱对照品适量，精密称定，加异丙醇-三氯甲烷（1：1）混合溶液分别制成每1ml含乌头碱50μg、次乌头碱和新乌头碱各0.15mg的混合溶液，即得。
Weigh accurately a quantity of aconitine CRS, hypaconitine CRS and mesaconitine CRS, respectively, dissolve in a mixture of isopropanol and chloroform (1 : 1) to produce a mixture containing 50 μg of aconitine and 150 μg of each of hypaconitine and mesaconitine per ml.

测定法 Assay

分别精密吸取对照品溶液与〔含量测定〕项下供试品溶液各10μl，注入液相色谱仪，测定，即得。
Inject accurately 10 μl of the reference solution and the test solution obtained under Assay, respectively, into the column, and calculate the content.

本品含双酯型生物碱以乌头碱（C34H47NO11）、次乌头碱（C33H45NO10）及新乌头碱（C33H45NO11）的总量计，不得过0.040%。
It contains not more than 0.040 per cent of the total amount of diester alkaloids, calculated as aconitine (C34H47NO11), hypaconitine (C33H45NO10) and mesaconitine (C33H45NO11) with reference to the dried drug.

含量测定 Assay

照高效液相色谱法（通则0512）测定。
Assay 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；以乙腈-四氢呋喃（25：15）为流动相A，以0.1mol/L醋酸铵溶液（每1000ml加冰醋酸0.5ml）为流动相B，按下表中的规定进行梯度洗脱；检测波长为235nm。理论板数按苯甲酰新乌头原碱峰计算应不低于2000。
Chromatographic system and system suitability Use octadecylsilane bonded silica gel as the stationary phase, a mixture of acetonitrile and tetrahydrofuran (25 : 15) as the mobile phase A and a 0.1 mol/L solution of ammonium acetate (add 0.5 ml glacial acetic acid in each 1000 ml solution) as the mobile phase B, elute in gradient as the following:

Time
(min) Mobile phase A

AS detector a spectrophotometer set at 235 nm. The number of theoretical plates of the column is not less than 2000, calculated with reference to the peak of benzoylmesaconitine.

对照品溶液的制备 Reference solution

取苯甲酰乌头原碱对照品、苯甲酰次乌头原碱对照品、苯甲酰新乌头原碱对照品适量，精密称定，加异丙醇-三氯甲烷（1：1）混合溶液制成每1ml含苯甲酰乌头原碱和苯甲酰次乌头原碱各50μg、苯甲酰新乌头原碱0.3mg的混合溶液，即得。
Weigh accurately a quantity of benzoylaconine CRS, benzoylhypaconitine CRS and benzoylmesaconine CRS, respectively, dissolve in a mixture of isopropanol and chloroform (1 : 1) to produce a mixture containing 50 μg of benzoylaconine and 300μg of each of benzoylhypaconitine and benzoylmesaconine per ml.

供试品溶液的制备 Test solution

取本品粉末（过三号筛）约2g，精密称定，置具塞锥形瓶中，加氨试液3ml，精密加入异丙醇-乙酸乙酯（1：1）混合溶液50ml，称定重量，超声处理（功率300W，频率40kHz；水温在25C以下）30分钟，放冷，再称定重量，用异丙醇-乙酸乙酯（1：1）混合溶液补足减失的重量，摇匀，滤过。精密量取续滤液25ml，40℃以下减压回收溶剂至干，残渣精密加入异丙醇-三氯甲烷（1：1）混合溶液3ml溶解，滤过，取续滤液，即得。
Weigh accurately 2 g of the powder (through No. 3 sieve) to a stoppered conical flask, add 3 ml of ammonia TS, accurately add 50 ml of a mixture of isopropanol and ethyl acetate (1 : 1) and weigh. Ultrasonicate (power 300 W, frequency 40 kHz, keeping the water temperature below 25℃)for 30 minutes, cool and weigh again, replenish the loss of the solvent with the above mixture, mix well and filter. Measure accurately 25 ml of the successive filtrate, recover the solvent to dryness in vacuum below 40℃,dissolve the residue in 3 ml of the above mixture, filter and use the successive filtrate as the test solution.

测定法 Assay

分别精密吸取对照品溶液与供试品溶液各10μl，注入液相色谱仪，测定，即得。
Inject accurately 10 μl of each of the reference solution and the test solution, respectively, into the column, and calculate the content.

本品按干燥品计算，含苯甲酰乌头原碱（C32H45NO10），苯甲酰次乌头原碱（C31H43NO9）及苯甲酰新乌头原碱（C31H43NO10）的总量应为0.070%～0.15%。
It contains not less than 0.070-0.15 per cent of the total amount of benzoylaconine (C32H45NO10) , benzoylhypaconitine (C31H43NO9) and benzoylmesaconine (C31H43NO10) , calculated with reference to the dried drug.

性味与归经 Property and Flavor

辛、苦，热；有毒。归心、肝、肾、脾经。
Hot；pungent and bitter. Meridian tropism: Heart, liver, kidney and spleen meridians.

功能与主治 Actions and Indications

祛风除湿，温经止痛。用于风寒湿痹，关节疼痛，心腹冷痛，寒疝作痛及麻醉止痛。
To dispel wind, remove dampness, warm the meridians and relieve pain. Indicated for wind-cold-dampness bi disorder, joint pain, cold pain in the heart and abdomen, pain in cold abdominal colic, and it can be applied for anesthesia to relieve pain.

用法与用量 Administration and dosage

1.5～3g，先煎、久煎。
1.5-3g. It should be decocted first for a long time.

注意 Precautions and Warnings

孕妇慎用；不宜与半夏、瓜蒌、瓜蒌子、瓜蒌皮、天花粉、川贝母、浙贝母、平贝母、伊贝母、湖北贝母、白蔹、白及同用。
Contraindicated for pregnant woman. Incompatible with Pinelliae Rhizoma, Trichosanthis Fructus, Trichosanthis Semen, Trichosanthis Pericarpium, Trichosanthis Radix, Fritillariae Cirrhosae Bulbus, Fritillariae Thunbergii Bulbus, Frifillariae Ussuriensis Bulbus, Fritillariae Pallidiflorae Bulbus, Fritillariae Hupehensis Bulbus, Ampelopsis Radix, and Bletillae Rhizoma.

贮藏 Storage

置通风干燥处，防蛀。
Preserve in a ventilated and dry place, and protect from moth.