Ketorolac Tromethamine CAS 74103-07-4 Maʻemaʻe >99.0% (HPLC)

Aia ka Ketorolac Tromethamine ma lalo o 98.5 pakeneka a ʻaʻole ʻoi aku ma mua o 101.5 pakeneka o C15H13NO3·C4H11NO3, i helu ʻia ma ke kumu maloʻo.
Hoʻopili ʻia a mālama ʻia - mālama ʻia i loko o nā pahu paʻa māmā.E kūʻai ma 25°, ʻae ʻia nā huakaʻi ma waena o 15° a me 30°
Nā kūlana hōʻike USP <11>-
USP Ketorolac Tromethamine RS
ʻike-
A: Infrared Absorption <197K>.
B: Ultraviolet Absorption <197U>-
Pane: 10 µg no mL
Medium: methanol.
C: Ho'āʻo Tromethamine-Hoʻomākaukau i kahi hopena maʻamau o USP Ketorolac Tromethamine RS i loko o kahi hui o dichloromethane a me ka methanol (2: 1) i loaʻa ka 5 mg no ka mL.E hoʻomākaukau like i kahi hopena hoʻāʻo o Ketorolac Tromethamine i loaʻa ka 5 mg no ka mL.E hoʻopili i nā puke 40-µL o ka hopena maʻamau a me ka hopena hoʻāʻo i kahi pā chromatographic ʻāpana lahilahi (e ʻike i ka Chromatography <621>) i uhi ʻia me kahi papa 0.25-mm o ka hui ʻana o ka chromatographic silica gel.E kau i ka pā i loko o kahi keʻena chromatographic i hoʻohālikelike mua ʻia me ka hui ʻana o ka dichloromethane, acetone, a me ka waikawa acetic glacial (95:5:2).E hoʻopaʻa i ke keʻena, a e hoʻomohala i ka chromatogram a hiki i ka neʻe ʻana o ka mea hoʻoheheʻe mua ma kahi o ʻekolu hapahā o ka lōʻihi o ka pā.Wehe i ka pā mai ke keʻena, a ʻae i ka solvent e mahu.E kāpīpī i ka pā me ka waiʻona hou i hoʻomākaukau ʻia me 30 mg ninhydrin no ka mL, a e wela i ka pā ma kahi o 150° no 2 a 5 mau minuke.Hoʻoulu ʻia nā kiko melemele me nā palena ʻulaʻula a i ka poni ma ka pā ma nā wahi i hoʻohana ʻia ai ka solution Standard a me ka solution test.
pH <791>: ma waena o 5.7 a me 6.7, ma kahi hoʻonā (1 i ka 100).
Nalo ma ka maloo <731>-Moloolo ia i loko o ka momi ma 60° no 3 mau hola: ʻaʻole e emi ma mua o 0.5% o kona kaumaha.
ʻO ke koena ma ka ʻā ʻana <281>: ʻaʻole ʻoi aku ma mua o 0.1%.
Nā metala kaumaha, Keʻano II <231>: 0.002%.
Chromatographic maemae-
ʻO ka pae kelepona, ka hui ʻana o Solvent, ka hoʻomākaukau maʻamau, ka hoʻonā hoʻonā, a me ka ʻōnaehana Chromatographic-E hoʻomau e like me ke kuhikuhi ʻana i ka Assay.
Hoʻoholo hoʻāʻo-E hoʻohana i ka hoʻomākaukau Assay.
Ke Kaʻina Hana-Chromatograph ka hoʻonā hoʻāʻo e like me ke kuhikuhi ʻana no ke Kaʻina hana i ka Assay, e ʻae ana i ka chromatography e hoʻonui i ʻekolu manawa o ka manawa paʻa o ketorolac.E ana i nā pane o nā piko a pau.E helu i ka pākēneka o kēlā me kēia haumia ma ka ʻāpana o Ketorolac Tromethamine i lawe ʻia e ke ʻano:
100rfi (ri / rs)
ʻo ia ka rfi ka pane pane o kēlā me kēia kiʻekiʻe haumia e pili ana i ka ketorolac;ʻO ri ka pane kiʻekiʻe no kēlā me kēia haumia;a ʻo rs ka huina o nā pane kiʻekiʻe a pau o nā piko haumia a me ka piko ketorolac nui.ʻO nā kumu kūʻai rfi he 0.52 no ka ketorolac 1-keto analog, 0.67 no ka ketorolac 1-hydroxy analog, 2.2 no ka peak haumia i loaʻa ka manawa paʻa o 0.54 e pili ana i ka ketorolac, a me 0.91 no ka peak haumia i kahi manawa paʻa pili. o 0.66.ʻAʻole i ʻoi aku ma mua o 0.1% o ka ketorolac 1-keto analog a i ʻole ka ketorolac 1-hydroxy analog i loaʻa;ʻaʻole i ʻoi aku ma mua o 0.5% o nā mea haumia ʻē aʻe;a ʻaʻole ʻoi aku ka nui o nā haumia a pau ma mua o 1.0%.
hoʻāʻo-
Mobile phase-Hoʻoheheʻe 5.75 g monobasic ammonium phosphate i 1000 mL o ka wai, a hoʻoponopono me ka phosphoric acid i kahi pH o 3.0.E hoʻomākaukau i kahi hui hoʻoheheʻe ʻia a hoʻoheheʻe ʻia o kēia hoʻonā pale a me ka tetrahydrofuran (70:30).E hana i nā hoʻololi inā pono (e ʻike i ka System Suitability ma lalo o Chromatography <621>) no ka loaʻa ʻana o ka manawa paʻa no ka ketorolac ma kahi o 8 a 12 mau minuke.
Mea hoʻoheheʻe wai-Hoʻomākaukau i kahi hui o ka wai a me ka tetrahydrofuran (70:30).
Hoʻomākaukau maʻamau-E hoʻoheheʻe i ka nui o ka USP Ketorolac Tromethamine RS i kaupaona pono ʻia i ka hui Solvent no ka loaʻa ʻana o kahi hopena i ʻike ʻia ma kahi o 0.4 mg no ka mL.[MAKUA-E pale i kēia hoʻonā mai ka mālamalama.]
Hoʻomākaukau hoʻāʻo-E hoʻoneʻe ma kahi o 20 mg o Ketorolac Tromethamine, i kaupaona pono ʻia, i kahi pahu volumetric 50-mL, e hoʻoheheʻe me ka hui Solvent i ka leo, a hui.[MAKUA-E pale i kēia hoʻonā mai ka mālamalama.]
Hoʻoholo hoʻoholo-I loko o kahi mea hoʻokaʻawale 250-mL e hui i 100 mL o ka wai, 100 mL o dichloromethane, 30 mg o USP Ketorolac Tromethamine RS, a me 1 mL o 1 N hydrochloric acid.E hoʻokomo i ka pahu, e lulu, a e ʻae i nā papa e kaʻawale.E hoʻololi i ka papa dichloromethane haʻahaʻa i loko o ka ipu aniani borosilicate i pani ʻia, a e hoʻolei i ka papa luna.E wehe i ka solution dichloromethane i ka lā no 10 a 15 mau minuke.E hoʻololi i 1.0 mL o ka hoʻonā i loko o kahi hue, e hoʻoheheʻe ʻia i loko o ke ʻano o ka ea a i ʻole i loko o kahi kahawai o ka nitrogen a maloʻo, hoʻohui i 1.0 mL o ka hui Solvent, a wili e hoʻoheheʻe.[NOTE-Hiki ke mālama ʻia kēia hopena ma lalo o ka pahu hau a hoʻohana ʻia inā lōʻihi ka chromatogram i loaʻa e like me ke kuhikuhi ʻia no ke Kaʻina hana kūpono no ka ʻike ʻana i nā piko ma muli o ke ketorolac 1-keto analog a me ketorolac 1-hydroxy analog, a no ke ana ʻana o ka hoʻonā. ma waena o ka ketorolac 1-keto analog a me ketorolac.]
Pūnaehana Chromatographic (e nānā i ka Chromatography <621>)—Ua hoʻolako ʻia ka chromatograph wai me kahi mea ʻike 313-nm a me kahi kolamu 4.6-mm × 25-cm i loaʻa iā 5-µm packing L7 a mālama ʻia ma kahi mahana mau ma kahi o 40°.ʻO ka nui o ke kahe ʻana he 1.5 mL i kēlā me kēia minuke.Chromatograph the Resolution solution, a e kakau i na pane kiekie e like me ke kuhikuhi ana no ke Kaʻina Hana: he 0.63 ka nui o na manawa paa no ka ketoroac 1-hydroxy analog, 0.89 no ke ketorolac 1-keto analog, a me 1.0 no ketorolac;a ʻo ka hoʻonā ʻana, R, ma waena o ke ketorolac 1-keto analog a me ketorolac ʻaʻole i emi iho ma mua o 1.5.Chromatograph i ka hoʻomākaukau maʻamau, a hoʻopaʻa i nā pane kiʻekiʻe e like me ke kuhikuhi ʻana no ke Kaʻina hana: ʻaʻole emi ke kolamu ma mua o 5500 mau papa theoretical;a ʻo ka ʻokoʻa maʻamau pili no ka hoʻopili hou ʻana ʻaʻole i ʻoi aku ma mua o 1.5%.
Kaʻina hana-Hoʻokaʻawale i nā puke like (ma kahi o 10 µL) o ka hoʻomākaukau maʻamau a me ka hoʻomākaukau ʻana i ka Assay i loko o ka chromatograph, e hoʻopaʻa i nā chromatograms, a ana i nā pane no nā piko nui.E helu i ka nui, ma mg, o C15H13NO3·C4H11NO3 i loko o ka hapa o Ketorolac Tromethamine i lawe ʻia e ke kumu:
50C(rU / rS)
i loko o ka C ka manaʻo, i ka mg per mL, o USP Ketorolac Tromethamine RS i ka hoʻomākaukau maʻamau;a ʻo rU a me rS nā pane ketorolac peak i loaʻa mai ka hoʻomākaukau Assay a me ka hoʻomākaukau maʻamau, kēlā me kēia.