Mai Xuan Tnidng vd Dig Tap chi KHOA HOC & CONG NGHE 118(04): 175- 178
DINH LU'ONG JDONG THOI PARACETAMOL, CHLOPHENIRAIMINE IMALEATE VA PHEIVYLEPHRINE HCl TRONG THUOC TIFFY BANG P m r O N G PHAP HPLC
Mai Xuan Tnrong , Vu Duy Long Trudng Dgi hgc Sir phgm - BH Thai Nguyen TOM TAT
Phucmg phap sac ky long hicu nang cao (High Performance Liquid Chromatography - HPLC) la phuong phap dem gian, chpn Ipc, nhanh chong, chinh xac va kinh le da dugc thuc hien de xac dinh dong ihdi paracetamol (PRC), chlopheniramine maleate (CPM) va phenylephrine HCl (PNH) trong cac dugc pham noi chung va thuoc TIFFY noi rieng bang each su dung pha dpng Ia hon hpp dem NaH3p04 0,05 M : acetonitrile (ty le th£ ti'ch la 93 : 07); Th§ ti'ch bcrm miu la 20 nL vdi toe dp dong chay pha dpng la 1,5 mL/phiit, sii dung loai cot C18, budc song do quang 215 nm va a nhiet dp la 30''C. Cac chit PRC, CPM, PNH Uong Ihuoc TIFFY da dugc xac dinh thanh cong vdi thdi gian Imi ciia PRC la 8,62 giay, thdi gian luu cua CPM la 2,78 giay va thdi gian luu ciia PNH la 3,27 giay. Hieu su3t thu h6i cua PRC la 99,7%; hieu suat thu h6i cua CPM la 99,5%; va hieu sudl thu h6i ciia PNH la 98,8%;.
Tu khoa: Paracetamol, chlopheniramine maleate, phenylephrine HCl, tiff)'. HPLC MO DAU
Phuong phap HPLC dugc thuc hien phd bien hien nay d cac trung tam kiem nghiem dugc pham do day la mdt trong nhirng phuong phap don gian, nhanh chdng, cd dp chfnh xac va do tin cay cao, phii hgp dc phan tfch thanh phan ciia thudc dudi dang vien nen.
Paracetamol (PRC) cd cong thiic pban Hi la CgHsOiN la loai thudc cd lac dung giam dau va ha sdt.
Chlopheniramine maleate (CPM) cd cdng diiic phan tu' la C16H19CIN2.C4H4O4 la loai thudc CO tac dung lam giam trieu chiing cua cam lanh thdng thudng va viem mui dj iing, vdi tinh chat an than.
Phenylephrine HCl (PNH) cd cdng thuc phan tu la C9H13NO2.HCI la mdt loai thudc giam xung huySt trong dieu tn benh viem miii dj ling theo mua va cam.
Cd nhiSu bai bao v^ phuang phap HPLC xac djnh rieng PRC, CPM va PNH nhung chua cd bao cao nao dinh Iugng dong thdi PRC, CPM va PNH trong thuoc vien nen ndi chung va thuoc TIFFY ndi rieng. Trong bai bao nay, chiing tdi thdng bao ket qua dinh luimg ddng thdi PRC, CPM va PNH trong thudc TIFFY theo phuong phap HPLC.
'Tel 0912739257. Emad truong/ihoahoa^gmailo
THUC NGHIEM Hoa chat va thuoc thir
Chat chuan paracetamol, chlopheniramine maleate va phenylephrine HCl nguyen chat do vien kiem ngbiem dugc san xuat.
Tbudc vicn nen TIFFY san xuat bdi cdng ty TNHH NACORN PATANA (Vict Nam, Sd 16:8936014420164; Ngay san xuat:
19/7/2013; Han sudung: 19/7/2018.
Natn dihidrophotphat, axil photphoric va acetonitrile linh khiet ciia Merck,
Nudc dung de pha hda chal la nudc cat 2 lan va khu ion.
Thiet bi va dieu kien sac ky
May s4c ky ldng hieu nang cao Hitachi L-2000 vdi detector UV-VIS L-2420 Cpt phan lich C18 (Inertsil ODS-3 250mm x 4,6).
Bo lgc dung mdi va mau vdi dudng kinh Id mang lgc 0,45pm
May lac sieu am, may do pH,
Pha ddng la hdn hgp dem diphotphat 0,05 M • acetonitrile (ly le Ih^ ifch 93 : 7).
Dem diphotphat duoc chuan bi bang each hoa tan 6,4g NaH2p04 trong 1 1ft nudc cat 2 lan
Mai Xuan Tmdng vd Dtg Tap chi KHOA HOC & CONG NGHE 118(04): 175-178 sau dd lac sieu am trong 10 phiit. Do pH cua
dung dich dugc dieu chinh bang 4,0 vdi axit photphoric thu dugc hdn hgp dem diphotphat 0,05 M. Pha hon hgp dem diphotphat 0,05 M va acetonitrile theo ty le 93:7 ve the tfch rdi lgc qua mang lgc 0,45 fim sau dd rung sieu am de khti bgt khf.
The tich bom mau la 20 |iL, tdc do ddng chay pha dgng 1,5 |iL/phiit d nhiet do BO^C, tin hieu dugc do quang tren detector UV-VIS L- 2420 tai budc song 215 nm.
Chuan bi cac mau chuan
Pba cac dung dich chuan CPM 2 (ig/mL;
PNH 7,5 ng/mL, va PRC 500 ^ig/mL trong binh dinh miic 25 mL bang hdn hgp nudc cat va dung dich pha loang vdi ti le ve the tfch la 24:1 (dung dich pba loang la dung dicb hon hgp dem diphotphat 0,05M: acetonitrile vdi li le ve the tfch la 1 : 1), Dung dich pha xong dugc rung sieu am va Igc qua mang lgc 0,45^m.
Chuan hi cac mau that
Can chi'nh xac 20 vjen ihudc TIFFY (moi vien cd chiia 500 mg PRC; 2 mg CPM va 7,5 mg PNH), sau dd Ifnh khdt lugng trung binb cua vien va nghien thanh bdt min. Can chfnh xac mgl tugng bpt thudc tuong duong vdi 100 mg PRC; 0,4 mg CPM va 1,5 mg PNH cho vao binh dinh miic 100 mL sau dd dinh mii'c bang dung dich pha loang va rung sieu am trong 15 phut, Hiit 12,5 mL dung dich vira pha vao binh dinh muc 25 mL va dinh muc bang dung dicb pha loang thu dugc dung dich cd chiia PRC 500 jig/mL; CPM 2 l^g/mL va PNH 7,5 (ig/mL. Lgc dung dich qua mang loc 0,45 \im.
K £ T QUA VA THAO LUAN
De chgn duoc pha ddng thfch hgp, chiing toi da tien hanh khao sat ti le thanh phan pha ddng la hon hgp dem NaHjPOA 0,05 M : acetonitrile d cac ty le vS Xhk tfch l§n lugt la:
85 ' 15 cho den 95 : 5. Su thay ddi tf le thanh phan pha dgng Iam thay ddi dang ke k6t qua sac ky Tuy nhien ty le hon hgp dem NaHzPO^ 0,05 M : acetonitrile 93 : 7 cho k6t
qua tdt nhat vdi thdi gian luu cua PRC la 8,62 giay, thdi gian lim cua CPM la 2,78 giay Va thdi gian Ixru ctia PNH la 3,27 giay. . ' Kiem tra tinh thich hgp cua h£ thong Viec khao sat tinh thfch hgp ciia he thdng sic ky dugc rien hanh qua viec tiem lap lai 6 ISn dung dich hdn hgp chuan de sic ki. Ket qua cbo thay chi sd RSD% cua dien tich pic va thdi gian luu dugc tim thSy trong gidi han cho phep (nhd hon 2%). Cac thdng sd he thong khac nhu sd pic ly thuyet va do phSn giai Cling nam trong gidi han cho phep. Vi vay he thdng sac ky dam bao tinh thich hgp vdi ca 3 chat phan tich.
Khao sat do tuyen tinh ciia phu'ong phap Do tuyen tinh dugc khao sat tren dung dich cac chat chuan vdi cac ndng do khac nhau:
PRC cd ndng do tir 400 - 800 ^g/mL; CPM CO ndng do tir 1 - 8 jig/mL va PNH cd nong do tir 5 - 50 pg/mL. Sau dd tien hanh chay sac ky Ian lugt tirng dung dich theo dieu kien sac ky da chgn d tren. Xac dinh dugc sir phu thupc tuyen tinh giira ndng do va dien tich pic bang phuong trinh hdi quy my6n tfnh va he so tuong quan. Ket qua khao sat cho thSy phuong trinh dudng hdi quy tuyen tinh ciia PRC la y - 9,67.10"^x - 34,83 vdi r^ = 0,999;
phuong trinh dudng hdi quy tuyen tfnh cua CPM la y = 7,74.10'^x - 0,14 vdi ^ = 0,999 va phuong trinh dudng hdi quy tuyen tinh ciia PNH la y = 9,30.10"^x - 0,38 vdi r^ = 0,999.
Xac dinh dong thdi PRC, CPM va PNH trong thudc TIFFY thu dugc phd dd nhu hinh 1, hinh 2, hinh 3 va bang 1.
Ket qua d bang 1 cho thay phuong phap HPLC xac djnh PRC, CPM va PNH co do chfnh xac va do thu hdi cao. Hieu suat thu hoi cua PRC la 99,7% hieu sudt thu h6i ciia CPM la 99,5% va hieu su^t thu hoi ciia PNH la 98,8%.
KET LUAN
Su dung phuong phap HPLC dinh Iugng d6i^
thdi paracetamol, chlopheniramine maleate va phenylephrine HCl trong thudc vien nen TIFFY cd do chinh xac, do thu hdi cao va co 176
Mai Xuan Trudng vd Dtg Tap chi KHOA HQC & CONG NGHE 118(04): 175- 178
the dimg de kiem nghiem chat lugng thuoc vdi ket qua chinh xac, nhanh chdng. Toan bd qua trinh phan tfch cd lh€ dugc thvrc hien frong vdng 10 phlil vdi viec su dung dung mdi don gian. Do dd, phuong phap nay phii hgp dk ap dung trong viec kiem soat chat lugng cua thudc da thanh phan tren thi trudng.
Hinh 1. Phd do cUa PRC
Hinh 2: Pho do ciia CPM
Hinh 3. Phd dd ciia PNH Bang 1. Ket qua X
ChSt Thai gian luu (phiit) Toe d9 bam mau {mUphiit) Di?n ticli pic (mAuxphut) Ham lugng (Bu/mU Bp thu hoi ( % )
c dink PRC, CPM v PRC 8,62
1,50 4613,9 498,60 99,7
CPM 2,7S 1,50 275.6 1,99 99,5
a PNH PNH 3,27 1,50 837,8 7,41 98,8
TAI LIEU THAM KHAO [1]. Anuradha S Jagtap, Savila S Yadav and Janhavi R Rao (2011), Simultaneous determination of paracetamol and lornoxicam by RP-HPLC in bulk and tablet fomulation.
Phamiacie Globale intemational journal of comprehensive pharmacy. 9, pp 1 - 4.
[2]. Dhara J.Patel, Vivek P.Patel (2010), Simultaneous Determination of paracetamol and Lornoxicam in Tablets hy Thin Layer Chromatography Combined with Densitometry, International Joumal of ChemTech Research, 2, pp 1929 - 1932 [3]. Katerina Milenkova, Aneta Dimitrovska.
Liljana Ugnnova, Suzana Trajkovi-Jolevsk (2003), Simultaneous determination of parecelamol. pseudoephedrine hudrochloride and dextromethorphan hydrobromide in tablets by HPLC, BulleUn ofthe Chemists and Technologists of Macedonia, 22, pp 33 - 37
[4]. M.Saeed Arayne, Najma sultana, Farhan Ahmed Siddiqui (2009), Simultaneous Determination of Paracetamol and orphenadrine citrate in Dosage Formulations and in Human Serum by RP-HPLC, Jour ofthe Chinese Chemical Society, 56, pp 169- 174
[5]. VK Redasani.AP Gorle ,R A Badhan. PS .Iain. SJ Surana (2013). Simultaneous
•.'eier..iiiiation of Chlorpheniramine maleate, phenylephrine hydrochloride, paracetamol and caffeine in pharmaceutical preparation hy RP- HPLC. Chemical Indusliy & Chemical Engineering Quarterly. 19. pp 57 - 65
Mai Xuan Trudng va Dtg Tap chi KHOA HOC & CONG NGHE 118(04): 175 -
S U M M A R Y
S I M U L T A N E O U S D E T E R M I N A T I O N O F P A R A C E T A M O L ,
C H L O P H E N I R A M I N E M A L E A T E A N D P H E N Y L E R P H I N E H C l I N T I F F Y M E D I C I N E B Y I I P L C M E T H O D
Mai Xuan Truong , Vu Duy Long College of Education - TNV Method of High Performance Liquid Chromatography (HPLC) is simple, selective, rapid, accurate and effective has been done to idenlily and paracetamol (PRC), chlopheniramine tnaleat (CPM) and phenylephrine HCl (PNH) in the pharmaceutical and medicine in general TIFFY using a mobile phase mixture of NaHiP04 0.05 M : acetonitrile (volume ratio 93 : 07); volume sample pump is 20 )j.L with a mobile phase flow rate of 1.5 mL/ min, using C I S column, measuring optical wavelength 215 nm and at a temperature of SO^C . The PRC quality, CPM and PNH in TIFFFY medicine has been successfully identified with the retention time ofthe PRC 8.62 second, the length ofthe CPM 2,78 seconds and the length of PNH 3.27 second. The recovery ofthe PRC is 99,7%; Recovery efficiency of CPM is 99,5%; and the recovery efficiency of PNH is 98.8%
Key words: Paracetamol, chlopheniramine maleate, phenylephrine HCl. Tiffy. HPLC.
Ngdy nhdn bdi 13/3/2014: Ngdy phdn bien: 15/3/2014: Ngdy duyet ddng: 25/3/2014 Phan bien khoa hoc: TS. Duang Thi Tii Anh - Tnrdng DH Suphgm - DH Thdi Nguyen
Tel 09I2~S925~, Email iruQngkhoahoa@gmaHcom
