Rp-hplc Method Of Determination - Chromatography - Education Industry - Butterfly Valve Manufacturer

Purpose By RP-HPLC method for the determination of related substances Balofloxacin

. Use SMTC18 column (250mm 4.6mm, 5 m), mobile phase of acetonitrile -0.4% sodium dodecyl sulfate solution (47:53) [with citric acid (1.5mol / L) adjusted pH value to 3.0], detection wavelength of 295nm, flow rate 1.0ml/min. Result Balofloxacin with all relevant material in the chromatographic separation conditions effectively. Conclusion The method is accurate, simple, sensitive and specific for determination of related substances Balofloxacin.

Balofloxacin (balofloxacin) by the Japanese Foreign Pharmacy Co., Ltd. and South Korea jointly developed Choongwae Fluoroquinolone, in 2002 for the first time in Korea [1 2]. Against Gram-positive bacteria, Gram-negative and anaerobic bacteria with broad-spectrum antimicrobial activity, selective inhibition of bacteria in vitro antibacterial activity of ciprofloxacin, ofloxacin and lomefloxacin 4 to 16 times [3]; and Tosufloxacin and sparfloxacin similar [4]. As in the parent nucleus Balofloxacin 8 introduces a methoxy, it not only increases the Gram-positive antibacterial activity, and avoid or reduce the light-sensitive or light toxicity and cell toxicity [5]. Balofloxacin is carboxylic acid ethyl ester as the starting material, the first and three-boron reaction of acetic acid chelate , and then, and 3 - methylaminopiperdine dihydrochloride condensation chelate , and then hydrolysis too. Preparation of the route is the optimal route Balofloxacin [6]. Determination of related substances commonly used Balofloxacin liquid chromatography, Yu Hong and [7] reported that the mobile phase with 0.05mol / L citric acid - acetonitrile (60:40) [triethylamine adjusted pH = 4] anti- phase liquid chromatography major intermediate carboxylic acid ethyl ester in the content Balofloxacin. The experimental conditions by exploring new chromatography, using acetonitrile -0.4% sodium dodecyl sulfate solution as mobile phase high performance liquid chromatography to the simultaneous determination of synthetic intermediates Balofloxacin carboxylate, chelate chelate complex and . The method is simple, accurate, good separation of the quality control Balofloxacin has obvious practical value. Balofloxacin and the intermediate structure shown in Figure 1.

1 Experimental section 1.1 Instruments and Reagent High Performance Liquid Chromatography ? Waters515 pump; 2487 UV detector. Balofloxacin samples made, batch samples: 20041015,20041020,20041024; reference substance made, content: 99.7%; carboxylate (Jiangyin Yongda Chemical industry Co., Ltd.), chelate , chelates were made; chromatography pure acetonitrile as reagent, other reagents were pure reagents.

1.2 Preparation of test solution for test solution: Take Balofloxacin (batch number: 20041024) approximately 10.2mg, home 100ml volumetric flask, add dissolved in mobile phase and diluted to the scale, shake, that was; intermediate solution: carboxylate 14.0mg, chelate 11.3mg, chelate 10.3mg, respectively for 100ml flask, add dissolved in mobile phase and diluted to the scale, shake, that was; mixed solution: the test sample intermediate solution and the solution of the 1, mixed, or have.

Figure 1 Balofloxacin and intermediate structure

Fig. 1 Structural formula of balofloxacin and intermediates

1 - Balofloxacin; 2 - carboxylic acid ethyl ester; 3 - chelate ; 4 - chelates 1.3 Chromatographic conditions Column: SMTC18 column (5 m, 4.6mm 250mm); mobile phase : acetonitrile -0.4% sodium dodecyl sulfate solution (47:53) [with citric acid (1.5mol / L) adjusted pH value to 3.0]; detection wavelength: 295nm; flow rate: 1.0ml/min; column temperature: at room temperature; injection volume: 20 l.

2 Results and discussion 2.1 Determination of Wavelength balofloxacin were weighed and the amount of intermediates were made of each solution add 1ml of acetonitrile containing 6 g about the solution, according to spectrophotometric method (Pharmacopoeia 2000 Edition 2 Appendix A), in 200 ~ 400nm The wavelength scan showed Balofloxacin the strongest absorption at 295nm Department, and other intermediates in the greater absorption near 295nm, 295nm-based products was chosen determination of related substances detected wavelength.

2.2 Column and mobile phase selection column: (1) DiamonsilTM C18 column (5 m, 4.6mm 200mm); (2) Kromasil C18 column (5 m, 4.6mm 200mm); (3) SMT C18 column (5 m, 4.6 mm 250mm). Mobile phase: (1) according to the Chinese Pharmacopoeia 2000 Edition 2 star drugs Sha determination of related substances, using mobile phase: acetonitrile-0.05mol / L citric acid solution (20:80) [adjusted with triethylamine to pH value to 3.5 ]; (2), acetonitrile? by 0.4% sodium dodecyl sulfate solution (47:53) [with citric acid (1.5mol / L) adjusted pH value to 3.0].

Using the different column and mobile phase experimental results show that: The column (1) or (2) and mobile phase (1), although the peak time of the main peak and the peak shape a better medium, However, the intermediate phase in this flow have not seen a peak 50min; with column (1) or (2) and mobile phase (2), the sample and the intermediate peak time was moderate, but severe peak tailing; use column (3) and mobile phase (2), peak time of the sample and the intermediate medium, and better peak shape. So choose column (3) and mobile phase (2) to test the goods related substances.

2.3 System suitability testing take 1.2 20 l solution were injected into the HPLC were determined and recorded chromatograms measured results in Table 1 and Figure 2. The results showed that: Balofloxacin with the intermediates in the chromatographic separation conditions effectively.

Table 1 Balofloxacin HPLC retention time with the intermediate

Tab.1 Chromatograms retention time of balofloxacin and relatedsubstances

Figure 2 Balofloxacin related substances HPLC system suitability test plan

Fig. 2 Chromatograms obtained from the system applicability test ofrelated substances in balofloxacin

1 - Chelate ; 2 - carboxylic acid ethyl ester; 3 - chelate ; 4 - Balofloxacin

by: gaga

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