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Trimebutine maleate tablets research and related substances determination

Time:2015/8/10 2:10:29

Abstract HPLC trimebutine maleate tablets and related substances were measured to octadecyl-bonded silica as a filler, 0.05mol / L potassium dihydrogen phosphate Myeong Gui translation? / FONT> 600: 300) with 1mol / L sodium hydroxide solution to adjust the pH to 5.0 as the mobile phase separation is good, with satisfactory results.

Maleic acid Trimebutine belong gastrointestinal motility drugs, the parties themselves in the Japanese Pharmacopoeia specifications pharmaceutical ingredient (1993 edition), Martindale Pharmacopoeia (1986 and 1992 edition 29 to 31) are close load. The measurement of related substances, Japanese Pharmacopoeia parties themselves pharmaceutical ingredient specification (1993 version) quality standards by HPLC with octadecyl bonded silica as a filler, perchloric acid solution (72% of the high acid 1.7 ml, dilute with water 2000ml, with 1% ammonium acetate solution to adjust pH to 3.0, plus pentane 0.1g of sodium dissolved, shake, that was) 椧 Gui translation? / FONT> 650: 350) as the mobile phase, the material and tablet Plymouth Hainan Pharmaceutical Co., Ltd. to provide testing, the results of the separation of impurities is not ideal. Change the selection by 0.05mol / L potassium dihydrogen phosphate Myeong Gui translation? / FONT> 600: 300) with 1mol / L sodium hydroxide solution to adjust the pH to 5.0 as the mobile phase, and by the stability test sample a variety of process conditions were measured, the results of the separation is better than the law.

1. Instruments and reagents

1.1 Instrument Waters501 pump 486 detector 746 digital processor

1.2 acetonitrile (HPLC grade, Shanghai Lu are industrial companies); and trimebutine maleate tablets, maleic acid, 2-dimethyl-amino-2-phenyl-butanol, 2-amino-2-phenyl butanol, 3,4,5-trimethoxy benzoic acid, 3,4,5-methoxybenzoate (above the sample and the reference provided by the Pharmaceutical Co., Ltd. Hainan Plymouth); other reagents were of analytical pure.

2. Experimental methods and results

2.1 Chromatographic conditions

Column: LichrosorbC18 (10μ, 4.6 × 200mm Dalian Berry chromatography center)

Detection wavelength: 254nm, flow rate: 1ml / min, the injection 20μl.

Mobile phase: 0.05mol / L potassium dihydrogen phosphate solution Myeong Gui translation? / FONT> 600: 300) and adjusted with 1mol / L sodium hydroxide solution to pH 5.0.

2.2 The minimum detectable amount and signal to noise ratio test from maleic acid Trimebutine amount, with 0.01mol / L hydrochloric acid solution / FONT> 13: 7) solution prepared solution containing 0.25,0.5,1μg per 1ml. Another 3,4,5-methoxybenzoate amount, with 0.01mol / L hydrochloric acid solution Myeong Gui translation? / FONT> 13: 7) produced per 1ml 0.05,0.1,0.2μg solution containing solution. Amount of the solution were each 20μl, into the liquid chromatograph, record the chromatograms. Results minimum detectable amount of maleic acid Trimebutine and 3,4,5-methoxybenzoate were 5ng and 1ng; SNR is 5.

Trimebutine maleate 2.3 of degradation was measured from maleic acid Trimebutine amount, plus methanol made solution containing 1mg per 1ml, placed five days. Amount of the above solution 20μl, into the liquid chromatograph, record the chromatograms. Results The main degradation products of 3,4,5-methoxybenzoate.

2.4 Determination results of samples

From maleic acid and sheet music United States pudding amount, plus 0.01mol / L hydrochloric acid solution / FONT> 13: 7) solution 1ml each containing 1mg for the test solution. Take 20μl, into the liquid chromatograph, record the chromatograms to 2 times the peak retention times. In addition to maleic acid peak, the sum of all impurity peaks area maleate and trimebutine peak area and comparing the peak area calculation, that is, too.