DOI:0.655/j.0254-793.20.09.039 75 * 2 2 3. 200435 2. 20203 3. 20000 ph R97 A 0254-793 20 09-75 - 05 Rapid Raman spectra identification and determination of levofloxacin hydrochloride injection * CHEN Bin ZHANG Shao - min YU Yue - lin CHEN Gui - liang 2 LE Jian 2 ZHANG Yu - min 3. Shanghai Zhabei Institute for Food and Drug Control Shanghai 200435 China 2. Shanghai Institute for Food and Drug Control Shanghai 20203 China 3. Shanghai Municipality Food and Drug Administration Shanghai 20000 China Abstract Objective To develop a method for the rapid identification test and determination of levofloxacin hydrochloride injection using Raman spectra. Method Raman spectra was used as the method of identifying testing and determination the levofloxacin hydrochloride injection. Results The result showed that the method of Raman spectra can identify the different of floxacin despinner levofloxacin and levofloxacin hydrochloride test ph of levofloxacin hydrochloride injection determinate the levofloxacin hydrochloride injection. Conclusion Owing to its fast and nondestructive properties the presented method can be developed as an analysis method for injection. Key words Raman spectra rapid identification and determination levofloxacin ofloxacin despinner identification 20 μm 2 ~ 0 * 20JY - 5 Tel 02 6683606 E - mail chenbin_zb@ smda. gov. cn
76 70 mg ml - ph. 52 ph 3. 4 ph 4. 87 ph 5. 8 ph 6. 05 ph 7. 05 ph 7. 68 ph 9. 08 ph 0. 29 ph. 48 3 4 Fig A B Structural formula of levofloxacin A and ofloxacin B Thermo Nicolet DXR near about 400 cm OMNIC - Agilent 00 30454-200403 00030 DK20-003273 0060 000 0002 0008 2 2. ph 7. 68 ph 9. 08 ph 0. 29 2 2 A 620 cm - B 400 cm - Fig 2 Raman spectra A near about 620 cm - B near about 400 cm -. levofloxacin 2. 3. ofloxacin 3 ph. 52 ~ 6. 05 ph. 52 ph 3. 4 ph 4. 87 ph 5. 8 ph 6. 05 A 620 cm - B 400 cm - Fig 3 Raman spectra of ph. 52-6. 05 from down to up ph. 52 ph 3. 4 ph 4. 87 ph 5. 8 ph 6. 05 A near about 620 cm - B 4 ph 7. 05 ~. 48 ph 7. 05 ph 7. 68 ph 9. 08 ph 0. 29 ph. 48 A 620 cm - B 400 cm - Fig 4 Raman spectra of ph 7. 05 ~. 48 from down to up ph 7. 05 B near about 400 cm - 2. 3 ph. 48 A near about 620 cm - 2. 3. 3. 92 53. 20 85. 0 06. 4 22. 5 mg ml - TQ 0. 9997 32. 92 ~ 22. 50 mg ml - 2. 3. 2 3 3. 20 mg ml - 2. 3. 3 2. 2 0
77 0. 60 mg ml - 2. 3. 4 0. 064 g L - 0060 6 000 0002 0. 30 mg ml - RSD 0. 98% 09. 50 98. 70 2. 3. 5 03. 60 mg ml - 0060 2. 3. 8 6 07. 20 mg ml - RSD. 3% 2. 3. 6 02. 30 mg ml - t 0060 5 ml 00 3 mg 3. 98. 7% RSD 2. 6% n = 5 Tab 2. 3. 7 3 0060 2 cm - Raman frequencies of ofloxacin levofloxacin and levofloxacin hydrochloride ofloxacin levofloxacin assignment 2999 m broad 3000 vw broad ν CH3 + ν CH2 2985 m broad 2962 m broad ν CH3 + ν CH2 2968 m broad ν CH3 + ν CH2 2949 m broad 2937 vw broad ν CH3 + ν CH2 2934 m broad 2934 m broad ν CH3 + ν CH2 2893 vw broad ν CH3 + ν CH2 2785 m broad 2803 vw broad 2856 m broad ν CH 79 w 728 w 79 w ν C = O OH 623 s 66 s 62 s ν C = O 547 sm 55 m 547 m ν C = C aromatic 59 m 536 m ν C = C aromatic 469 m 467 m δ CH + δ CH2 + δ CH3 + ν 455 m 45 m δ CH + δ CH2 + δ CH3 + ν 442 m 438 s δ CH + δ CH2 + δ CH3 + 399 s 40 s 40 s δ OH 355 w 359 m 352 m biforked δ CH + δ CH2 + δ CH3 342 δ CH + δ CH2 + δ CH3 325 w 33 m 39 w ν CN 287 w 296 w δ CH + δ CH2 + δ CH3 + ν 257 w δ CH + δ CH2 + δ CH3 + ν 236 w ν C - O 227 w ν C - O 208 w 206 w ν C - O 99 w 9 w ν C - O 72 w ν C - N 62 w ν C - N 45 w 4 w ν C - N
78 ofloxacin levofloxacin assignment 29 w 5 ν C - N 072 w 090 w ν C - N 057 04 050 ν C - N + ρ CH2 039 m 030 m ν C - N + ρ CH2 00 00 ν C - N + ρ CH2 983 988 985 ν C - N + ρ CH2 893 m 905 m ν C - N + ρ CH2 889 ν C - N + ρ CH2 852 835 848 ν C - N + ρ CH2 798 ν C - N + ρ CH2 786 m 783 m 783 m ν C - N + ρ CH2 750 749 746 ν C - N + ρ CH2 709 ν C - N + ρ CH2 688 ν CH + δ CH 670 668 663 ν CH + δ CH 653 645 ν CH + δ CH 599 596 δ cyclo + δ CH 569 560 567 δ cyclo + δ CH 548 547 538 δ cyclo + δ CH 504 486 49 δ cyclo + δ CH note ν - stretch vibration δ - bent vibration s - stong peak m - medium intensity peak w - weak peak 2999 2986 2967 2949 cm - CH 3 CH 2 2786 cm - CH 79 cm - C = 3000 cm - CH 3 CH 2 O 623 cm - C = O 623 2999 2985 2968 2934 cm - cm - 469 455 442 287 257 cm - CH 547 cm - CH 2 CH 3 C - H 236 59 cm - 2 455 227 208 99 C - O 355 287 257 cm - CH 3 CH 2 72 62 45 29 C - N 325 cm - 889 798 CH 2 709 C - N 236 227 99 cm - C - O 45 072 cm - 2 057 039 00 983 893 852 786 750 709 cm - C - N CH 2 C - H C - N 688 599CH CH 3. 2 2 599 569 548 504 cm - CH CH 2 A 2 2 B C CH 3 H 2 C D
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