Process for separating and determining pregabalin/Lyrica chiral isomer
A chiral isomer, pregabalin technology, applied in the field of analytical chemistry, can solve problems such as high cost and difficult separation, and achieve the effects of fast reaction speed, high analytical sensitivity, and stable derivatized products
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Embodiment 1
[0031] Instruments and Conditions
[0032] U.S. Agilent 1100 high performance liquid chromatography system and workstation; automatic sampling; chromatographic column adopts octadecylsilane bonded silica gel column; ultraviolet detection wavelength: 340nm; mobile phase: triethylamine solution (take 5ml of triethylamine, add water 1000ml, adjust the pH value to 3.0 with phosphoric acid solution)-acetonitrile (55:45).
[0033] Experimental procedure
[0034] Take about 160 mg of the racemate of pregabalin into a 10 ml measuring bottle, take an appropriate amount of 1 mol / L hydrochloric acid solution, shake to dissolve, neutralize with 1 mol / L sodium hydroxide solution, and dilute to the mark with water. Shake well as a sample solution; take another 10.0 mg of Nα-(5-fluoro-2,4-dinitrophenyl)-L-alanamine amide, add 1 ml of acetone, shake well, and use it as a derivatization reagent solution. Take 50 μl of sample solution, 200 μl of derivatization reagent solution and 20 μl of 1m...
Embodiment 2
[0037] Get about 80mg of pregabalin to 10ml measuring bottle, prepare need testing solution according to the experimental procedure of embodiment 1 below, and carry out high performance liquid chromatography analysis under the condition of embodiment 1, the results are shown in Figure 3.
[0038]The chromatographic peak of retention time 3.666 minutes among Fig. 3 is excess derivatization reagent peak; configuration, 0.5%) of the chromatographic peaks. Figure 3 shows that pregabalin and its chiral isomers and excess derivatization reagents can achieve baseline separation, and can accurately determine the chiral isomer impurities contained in pregabalin.
Embodiment 3
[0040] Get an appropriate amount of pregabalin capsule content (approximately equivalent to 80 mg of pregabalin) in a 10ml measuring bottle, prepare the test solution according to the experimental procedure of Example 1 below, and carry out high performance liquid chromatography analysis by the conditions of Example 1 , the results are shown in Figure 4.
[0041] The chromatographic peak with a retention time of 3.633 minutes in Fig. 4 is the peak of excess derivatization reagent; the chromatographic peak with a retention time of 8.116 minutes is the chromatographic peak of pregabalin. Figure 4 shows that pregabalin and excess derivatization reagent can achieve baseline separation, if the sample contains pregabalin chiral isomer impurity, it can be accurately determined by this method.
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