《日本药局方第十八修正(JP18)》数据分享-1

拉呋替丁有关物质

拉呋替丁为胃溃疡治疗药物，日本药典中规定“理论塔板数8000以上，拖尾因子1.5以下”。使用CAPCELLPAK C18 MGIIS5（4.6mmi.d. x150 mm）色谱柱，得到了理论塔板数12100，拖尾因子0.9的良好分析结果。　

拉呋替丁(10mg/mL)

Lafutidine (M.W. 431.5)

【HPLC Conditions】

Column: CAPCELL PAK C18 MGII S5; 4.6x150

Mobilephase: Dissolve0.87 g of sodium 1-pentanesulfonate to 1000 mL of diluted phosphoric acid (1 in 1000). To 850 mL of this solution add150 mL of acetonitrile.

Flowrate: 1.2 mL/min

Temperature: 40 ˚C

Detection: UV 220 nm

Inj.vol.: 5 μL

Sampledissolved in: Mobilephase

※1 mg/mL = 1 ppm

法莫替丁注射液含量测定

法莫替丁为胃酸抑制药物，日本药典中规定“按照法莫替丁、内标物质的顺序出峰，分离度达到26以上”。使用CAPCELLPAK C18 AQS5（4.6mm i.d. x150 mm）色谱柱，可得到分离度为27.2 的良好分离结果。

法莫替丁(100 mg/mL)

Famotidine(M.W. 337.4)

尼泊金甲酯(I.S.) (20 mg/mL)

Methylp-Hydroxybenzoate(I.S.) 

(M.W. 152.2)

【HPLCConditions】

Column: CAPCELLPAK C18 AQ S5; 4.6x150

Mobilephase: To 900 mLof water add 1.74 g of sodium1-pentanesulfonate, adjustto pH 4.0 with diluted acetic acid (1 in 10), and add water to make 1000 mL.To 750 mL of this solution add 200 mL of methanol and 50 mL of acetonitrile.

Flowrate: 1.3 mL/min

Temperature: 40 ˚C

Detection: UV 254 nm

Inj.vol.: 10 μL

Sampledissolved in: Prepared according to theJapanese Pharmacopoeia

※1 mg/mL = 1 ppm

法莫替丁片含量测定

法莫替丁为胃酸抑制药物，日本药典中规定“按照法莫替丁、内标物质的顺序出峰，分离度达到11以上”。使用CAPCELLPAK C18 MGIIS5（4.6mm i.d. x150 mm）色谱柱，得到分离度为16.7 的良好分离结果。　

法莫替丁(100 mg/mL)

Famotidine(M.W. 337.4)

尼泊金甲酯(I.S.) (20 mg/mL)

Methylp-Hydroxybenzoate(I.S.)

(M.W. 152.2)

【HPLCConditions】

Column: CAPCELLPAK C18 MGII S5; 4.6x150

Mobilephase: To 900 mLof water add 2.0 g of sodium1-heptanesulfonate, adjustto pH 3.0 with acetic acid, and add water to make 1000 mL.Add 240 mL of acetonitrile and 40 mL of methanol to this solution.

Flowrate: 1.25 mL/min

Temperature: 25 ˚C

Detection: UV 254 nm

Inj.vol.: 5 μL

Sampledissolved in: Prepared according to theJapanese Pharmacopoeia

※1 mg/mL = 1 ppm

头孢氨苄有关物质

头孢氨苄为头孢类抗生素药物，日本药典中规定“理论塔板数150000以上，拖尾因子0.8-1.3之间”。使用CAPCELLPAK C18 MGIIS5（4.6mm i.d. x250 mm）色谱柱，得到理论塔板数292000，拖尾因子1.1 的良好分析结果。　

头孢氨苄(20mg/mL)

Cefalexin (M.W. 347.4)

【HPLCConditions】

Column: CAPCELL PAK C18 MGII S5; 4.6x250

Mobilephase:

A)Dissolve 1.0 g of sodium 1-pentanesulfonate in 1000 mL of water,add 15 mL of triethylamine, andadjust to pH 2.5 with phosphoric acid.

B)Dissolve 1.0 g of sodium 1-pentanesulfonate in 300 mL of water, add 15 mL of triethylamine, andadjust to pH 2.5 with phosphoricacid. To this solution add 350 mL ofmethanol and 350mL of acetonitrile.

B 0%(0 min)-0%(1 min)-100%(34.5 min)-100%(35.5min)-0%(35.6 min) Gradient

Flowrate: 1 mL/min

Temperature: 40 ˚C

Detection: UV 210 nm

Inj.vol.: 20 μL

Sampledissolved in: Preparedaccording to the Japanese Pharmacopoeia

※ 1 mg/mL = 1 ppm

头孢氨苄胶囊含量测定

日本药典中规定“按照头孢氨苄、内标物质的顺序出峰，分离度达到8.0以上”。使用CAPCELLPAK C18 MGIIS3（3.0mm i.d. x 75mm）色谱柱，得到分离度为13.0 的良好分离结果。　

头孢氨苄(20mg/mL)

Cefalexin (M.W. 347.4)

3-羟基苯乙酮(I.S.) (6.7mg/mL)

3-Hydroxyacetophenone (I.S.)

(M.W.136.2)

【HPLCConditions】

Column: CAPCELL PAK C18 MGII S3; 3.0x75

Mobilephase: Dissolve 2.7 g of monobasicpotassium phosphate in 1000 mL of waterand adjust to pH 3.0 with diluted phosphoric acid (3 in 500).To800 mL of this solution add 200 mL ofmethanol.  

Flowrate: 0.5 mL/min

Temperature: 25 ˚C

Detection: UV 254 nm

Inj.vol.: 10 μL

Sampledissolved in: Preparedaccording to the Japanese Pharmacopoeia

※ 1 mg/mL = 1 ppm

头孢妥仑匹酯含量测定

头孢妥仑匹酯为头孢类抗生素，日本药典中规定“按照内标物质、头孢妥仑匹酯的顺序出峰，分离度达到5以上”。药典中要求使用乙腈作为溶剂，但由于溶剂效应导致峰型异常，因此我们将溶剂更换为了50%乙腈，在此条件下使用CAPCELLPAK C18 MGIIS5（4.6mm i.d. x250 mm）色谱柱，得到分离度为8.3 的良好分离结果。

尼泊金丙酯(I.S.)(500 mg/mL)

Propylp-Hydroxybenzoate(I.S.)

(M.W. 180.2)

头孢妥仑匹酯(400mg/mL)

CefditorenPivoxil(M.W. 620.7)

【HPLCConditions】

Column: CAPCELLPAK C18 MGII S5; 4.6x250

Mobilephase: Dissolve0.79 g of ammonium formatein 500 mL of water and adjustto pH 6.0 with formic acid. To 450 mL of this solution add 250mL of methanol and 250 mL of acetonitrile.

Flowrate: 0.99 mL/min

Temperature: 25 ˚C

Detection: UV 230 nm

Inj.vol.: 10 μL

Sampledissolved in: 50 vol% CH3CN

※1 mg/mL = 1 ppm

《日本药局方第十八修正(JP18)》

拉呋替丁有关物质分析推荐用柱

F92532 CAPCELL PAK C18 MGII S5; 4.6x150

法莫替丁注射液含量测定推荐用柱

F92044 CAPCELLPAK C18 AQ S5; 4.6x150

法莫替丁片含量测定推荐用柱

F92532 CAPCELLPAK C18 MGII S5; 4.6x150

头孢氨苄有关物质分析推荐用柱

F92533 CAPCELL PAK C18 MGII S5; 4.6x250

头孢氨苄胶囊含量测定推荐用柱

F92474 CAPCELL PAK C18 MGII S3; 3.0x75

头孢妥仑匹酯含量测定推荐用柱

F92533 CAPCELLPAK C18 MGII S5; 4.6x250