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    woueeuneteu UOC TAR BOY TE VIRN KIEM NGHIEM THUOC TP. HO CHE MINH ‘Bia chi: 200 CO BAG, P. CO GIANG, QUAN 1 ‘ign thogi: 028 3836 8518 ~ 028 38374802 Email: hdt@vienkiewmghiem.gov.vn Website: ww. vienkiennghiemgov.on Tai ligu dao tao THAM BINH QUY TRINH PHAN TiCH (14 QR a tip nh phn hi, rao abi thing tn Top he) Minh, nim 2022 ‘Thanh phé Hi en eunoneu nese eva CHUONG TRINH DAO TAO “THAM BINH QUY TRINH PHAN TICH” (0 gan: 231022023 ti Vign Kl ng thube Tp. Chi Mink) “Thi gian Noi dung Ging view Bui ing 8:00-8:45 _|- Tip oe vien vp gw Phang Khoa hoe & Dao eo 45—9.00 |-Kiwimee Kp hoe yl ifn Bon lh do = Yeu cco bin rong Thm dish aoy TS. Ha Minh én 3,00-9:45 |" wah pin eh theo ICH Q2 (81) vA | (Trudng Phong Khoa he & Inudng din GLPAWHO, Asean hig hin Dow 9345—10:00 |= Gititeo = Yeu cha chung v8 tne shea guy tinh 1» | thin pags pp phan eh vsinh | TS. Pham Thi Minh Tam 1000-1130 | ging a hit guy tn this dh 1 | (rang Khoa Vi sinh ben iu visio, a Bult edu | “Thim dink quy wih pong pp pain] TS. HA Moh Hin 1330-1445 | gh dang ev Thing sco bin vie | ctyyéng Ping Khoa hoe & nit guy ten io te0) nets—15:00 |. Gidilao | Thi dink uy wink pin ch phvong | TS. Ha Minh Hib 1500-16: |” pap hoa: Thang sco tan v8 ne | crrubng Pag Khoa be & nit quytenh Biot) trae dB. thio ato Giang vin 161-10 | Bk ae Phang Khoa hoe & Bio 10 ‘WEN KEM NGHEM TAUB TC vin KIEM NGHIEM THUGC yYéu CAU CO BAN TRONG THAM BINH QUY TRINH PHAN TECH THEO ICH Q2 (Ri) & HUGNG DAN GLP-WHO, ASEAN HM, Hin 2023 Dude si ae 00% Duc? thusc va nguyén liu tam thud quat gigs ‘len aEMNHEW THUD TeHEM GrAI THICH TU NGO ‘Binh nghfa thu + Tule ten pn co cna edt hte deen cho nat = Pig bon fol = ef ain ih 7p) = com tean = pau oe = Gli be bah = i ean ing nh ots + Thus tao gs “Techie duce Luat Duroc 2016 Tre ue Hue rato + Wea vi i pin 4 GIAL THiCH TU New Now tn tae th po tam ia vo cto ciate bo im Gage chit, dae Ku, 18 cage, wb nang ge st dung rong gu tc sn st hue. EEE ee Peon aeten sci Pi ser tema bek toy Prise os gyre anes ute ay Pia iprtraa enna Ens sini ysiia ure Huby ecas tah ‘Du fe Ba nauyén iu lm ude e& noun of {urnhin ite vt, ag vi Kong vv dt ‘iu en tam tue ‘Wen Kg NGM THUGS THC GIAI THICH TU NGO Noun btm ace than phn ham i vo eu tg ca Woe bao gm doe chit, due i,t ete, vb nang de si dung trong qua rah sin st tte, GIAI THiCH TU NGO’ Mush de cca as cit | poecpos : (Gon woe dons Eanivatenc) *: Chi cé & EPIBP,®: Chicé & USP: bi vi phuong pip hay th cl uu ee thong 8 thm din ea phuong pip thay {ng phi ph op vi yeu chu v8 mae chit twgng vi sin wong mu thir eta phuong php ‘ieu chun a en aga nonteuritube Tee 2. Phueong pip this jah 21 Thim dink phiwong php Xée dink hogt le khang sink bing phuwong phip vi sinh 21 Phuong phép Khuéeh tin 6 je higu: Chun bj ede mau placebo, méu chun, miu placebo them chun theo quy tinh a8 xay ‘dung. Do during kinh ving khsing khudn eta ee miu placebo, man chun vi miu placebo thém chuan khang sinh (v6i nding 4 bing néng 4 khéng sinh trong mau chun). [ing Kg sinh ge chon nén phi hop vi ning 69 di wEME. a Gls oOAL ign trong ce miu 1-tegt placebo, placebo thém chun va miu chun, Phuong phép c6 tinh dc higu khi miu ‘Banh gid bing efch nbn biét va so sinh vng khng khudn wait placebo khéng ¢6 véng khing khudn, dzimg kinh vong khéng khudn cia miu chudn vi smu placebo thm chuén (cing néng d9) kh nhaw khdng ¢6 y nghia théng ke. hosing tuyén tn: Pha long Khng ssh chun thinh dy eée ning 9 Khe hau va do diving kinh ving King Kin oa ee ng 9 ny. Te, vé dng i quy tuyén tah tao bai logarit ndng dd khing sinh va dng kth vang King Khun tong ing. Chon khodng nang d6 tmyén tinh ma R? > 0,95, DSi v6i phuong phip tigu chun, e6 thé chon i thigw Sng 4 sao cho phd hékhodng ndng ch tn din ang ly theo pong Bee ob UVa phip si dung pong php thng ke ay huang phi dung chubn). A+ i oun Thy hign bing pong php thm chun vo mu placebo, Néng chin them vio thudng 63 mic 9, 100, 120% so vi him ugng nh, MBF mie ning 6 the én 3m Ge tp, Xie dh 6 thu hb ea tng thi nin ‘DG ehinh xée: Xée dinh aS chinh xde pha thge hign tren cong mot miu tar dng nnd, 1ip la 6 lin de lip. BS ehfnh xéec trong gian pha the ién 6 Hin de jp tuong ty bai ich khde, C6 thé dn gid 49 lp Ii eda mi kim nghigm vien bing gid n ing test (s0 sini 2 s6 tung, mt nau phi tu RSD va inh gi Kt qui gta 2 kid nghign vi nly, Cing 66 thé in it kk qua theo phone psp xe din toh dng nh ia fe a le Wate HOE TE ‘két qua thirnghigm, Duge dién Vigt Nam V, Phy lye 13.10, mye 4 : Phéi hop ede két qua thirmghigm, 2.1.2 Phinomg php do a6 due 42 Thim djnh tuong ty nue phuong php khuéch tén, R? trong phuong phip niy > 0,90, Luu ¥ mdi dng thir nghiém trong phuong phép do 46 dyc 1a mOt thir nghiém dc lap. 2.2 Phuong php xie duh cic thing sb rong thm dink ede phung php vi sinh 22.1 Thim dn kha ning phe hd Recovery) ‘Thim dinh kha nang phye hdi duge ding trong thém dinh phi hgp eda cée phusong phip ésn'xée din sy ¢6 mat vi sinh VBC trong ede thir nghigm Gigi han nhim kh, Thi hhigu qua kldng khuén chét bio quin, dinh lugng probioties/LBP va thir BQ v6 khuan. Ki ing phy Bai vi ‘tra Khem thi (remove) va trang hd hoa tin Kn Khun (nd 6) tong mn tht inh trong mu thir ién quan én vige ich chiét duge ee vi sinh (neutralizing). 2.2.1.1 Phuong php rung hoavtogi bo hogt tinh khing Khun Dé loi bs hop nh King Khun: 6h dng phuong php pha fons, phuons ‘hap Ige va hoge phuong phip ding ee chit tung hoa Pharong php ding ehde rng da ‘Bang 3 win by mot s6 chit rung hd va Ka nding de hd ee vi sinh vat ey thé. Thube [khing sinh Kh 6 th8 trong hda bing phuona php hang, 6 thé xt bing enzyon (M1 «ly mu thio king sinh dhugenhém Pelatam, cephalosporin e6 thé ding peniilinase/ cephalosporinase dé trung hia). Bang 3. Mot s6 chit trung hoa (cit kaking kuin cha nang te end [Bisulfite [Glutaraldehyde, Mercurial Vi khuin Khang bio tr 2 ‘veaéienanteu ude TH [chat trang nda [Chat khang Khun [ch ning ite eh [Difation [Phenolies, Alcohol, Aldehydes, [= \Sorbate (Giveine [Aldehydes |Vi khudn dang dvong bao [cesta [Quaternary Ammonium Compounds [Vi Khuin lroacs, Parabens, Bis-biguanides [vig'2 or Cav2 ions|EDTA = Polysorbate JQACS, Todine, Parabens | - HThioglycollate _ [Mereurials [Staphylococet, bio tr FThiosulfare |Mercurals, Halogens, Aldehydes [Staphylococci Pinca pp pha Ting (C6 thé tam mit ed je tinh Khéng kun eta sin phim bing phuong php pha lang, v tihng da cht dig kuin ha hoe 6 hing Kn én hig pe ca ns. Mi quan be ita ning dd va te dong king kuin Khe nhau gta ef ct dig khan nung King 90% BG lech duong |biar) |< 10% BO Iecham | eiferd) ‘Tinh dje higu ota phuong php dinh tnh/dinh Iugng thay thé 1a kha nding chi phat hign vi sinh vt ci i, te dng tgora kt qua ong inh gi. Ching msn ing ch sic vi sin Vt th 6) va xée dinh x2 (0.05, N 1). D8 chin xe ‘Mie di m6i quan he gita 2 két qua durge mong doi ta tuyén tinh, tuy nbign quan he -khéng tayén tinh vn duge chp nn néu ching minh sy twomg quan Spearman thay cho ‘ong quan Pearson. 2.2.9 BG tin efy/BS ving: stn cdy dug ne dn ing cch dn it so sh Kt qua hi 6s Khe hau v2 eke thang sb cia phon phi. Vie doh gid tn cy nén duge xem xh nghién ea sy dmg guy tinh, NE kt qu thi gin bj thay Bib yu 6 no, ht phi ibn soit yéut6 6p hop ode pa a vo hr tong uy tn Ty nig, néu ee thong si quan tong bi thay iti Bt nh rng no én tin ey a phi id, B§ tin efy eli phuromg php dinh tinh duge dn gi bing kha nang phat hign cde vi fuge din n sau kh thay dBi 06 chi ¥ di vi ee théng 54 eda phurong php sinh vt thir mh _Dé tn edy eda phrong phap din Irgng thay thé duge dénh gid ing kha nding dm chink sxe fe vi sinh vt sau ec thay di c6 cha ¥ ede thong s6 eta phusong php. 2.2.10 D6 chi ehin/ D6 thé: Buge dénh gid nh chink wée rung gian 2.2.11 Tiah phit hop ea eta phuong php (Suitably): _p4i v6i phuomg phép dinh tnh/ajnh Kwong, tinh pha gp pha chung minh duge ring miu thr nghigm king anh hudng dé kha nang phat hign/dém vi sinh vat eda he théng hose kh ming phe hai vi sinh vit (xem 2.2.1). Cae diém cy thé cd gid quyt i (Qk sng i pig wi si toe Bia dgn ee mae as a uno None Tauoe THe (cha nang nen mu €6 ean we phuong php thir hay khong (vi du: tin higu nén hoe phin ling ha ie ech. 2.2.12 Khodng xe doh Range) Pham vieja mot phuong php din long thay thé li khsing gta me én va mie di cia vi sinh vt de xe dinh re nghign et itn quan v8 dinh xe, 9 ing v tinh twyén in bing pom php 4 chi din ving dng dr oh ‘Tai ifu tham Kho USP - General Chapters: <1227> Validation of microbial recovery from pharmacopeial articles. USP-General Chapters: <1223> Validati LUSP-General Chapters: <1225> Validation of compendial procedures. of alternative microbiological method. LUSP-General Chapters: <1226> Verification of eompendial procedures LUSP-General Chapters: <61> Microbiological examination of nonstrile products: Microbial enumeration tests EPIBP-SC IV. Altemative Methods for Control of Microbiological Quality 180 16140-3:2 for the verifea Inboratory, 1: Mierabiology of the food chain- Method validation- Part 3: Protocol of reference methods and validation alterative methods ina single ICH Topie Q 2 (R1): Validation of Analytical Procedures: Text and Methodology. NATA-Guidelines for the validation and verification of quantitative and qualitative test methods, ‘Trin Cao Son- Vign kiém nghigm an toan v@ sinh thye phim quée gia- Thm dint phwong php tong phn tich héa hoe va vi sinh vat 2 2023-02-21 ‘entre te re EX pee SS Method validation ICH Q2 (R1) InereationalCanereee cn Harmonisation IC. The objective of any analytical determination is to obtain consistent, accurate and reliable data. 2023-02-23 Method validation process The validity of a specific method should be demonstrated in laboratory The samples or standards being used for the validation should be similar to unknown samples which will be analyzed routinely. 2023-02-21 Instrument goaification During method validation, parameters and acceptance criteria for system suitability checks and quality control checks are defined. Validation protocol Acceptance citer shouldbe integrated int the roto An assay category isselacted Tr Wenteation et 2: Quantfiaton of impurities 8-Quanttatielimi test or Impurities 1 Asay of APL 2023-02-23 Validation parameters required for the choosen category must be included in the analytical method validation protocol. Assay Category Talon parameters equlted for at category are chon, ese crayeg 108 a Cee 2023-02-21 ‘xamplssAceptance tera fra mathod being wed for identiiestion of nelamin fm povodon ponders | stamens cima. 2023-02-21 322, Precision The precision of the method was evaluated by anavaing four samples containing the solutes stifferen concentrations (Seton 312) The intermediate precision wie determined ver four days {ted6) and indifferent capillaries by performing atleast twelve sucessive daly nection. The relative standard deviations (RSD) éFinta-day and inter-ay analyses were determined oe apr tmitely0.383nd358forthemigration times and 003 snd 0.0% or {heltive migration tmeSyndieating excelent precision, able 2 “The esi eporTT Table? and iz. > demonstrated thatthe SDS Ines were able to resolve any interference between poidone, present ata very high concentation (20mg) andthe sles {rot The restits aso showed that neither the absolute no lative tnigration times were aflected by the solute concentration, abe? (Tet [lial procedire | Aceplance citi Appearance | Wivalispcton | Cmplis ideniy eit mpg Cope Tey ee Gonpes| tet aE = ah Reed NS mea a Taopicinpies | PAC my Topobc mpeg —_—_[PIRE _ ib ig cnr Weis | CC) = Tesson Drying Dying ar acral Edotonns Kinetic chromogenic mead, PRE | Across the range of LOQ-150% of the target concentration (shelf life limit), -5 concentrations, in ‘tiplicate each. (LOQ, 50%, 100%, 150%) > Percent recovery: in general, within 80-120%, depends on the level of limit Accuracy Impurities (Quantification) aunt: or 2023-02-21 Impurituies are not available Compare the test results of samples containg impurities/ degradation products to a second well characterized procedure. RF (response factor) is the response (e.g. peak area) of an analyte per unit weight, i.e., RF = Peak area/ [Analyte] RRF = RF inpurity / RFavi or RRF = Slope impusity/ SIOPe ari x 2023-02-21 1,2>RRF>0.8 no correction is necessary Correction factor = 1/RRE (the reciprocal of the RRF) ‘When using APL a the erence RF should bo used rjastifestion of ‘icon shoul be provided (Qvcetecretoneleconotsnpio) Recommended data (ICH 2QB) “Accuracy is assessed peroforming a minimum of 9 determinations over a3 concentration levels covering the specified range. “It is reported as percent recovery. a 2023-02-21 5. precision ICH: precision is defined as the closeness of agreement (degree of scatter) between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions. Precision may be considered at three levels: repeatability, intermediate precision and reproducibility. 5.1.Repeatability Tice erent 0 serge OF Anan ft sinew °F emmemmoar 00% Preven 2023-02-21 ' aE rst 7 Precision. Repeatability (method precision) = Multiple measurements of a sample by the same analyst, = A minimum of 6 determinations at the test concentration (6 times of a single batch), or ~3 levels (80%, 100%, 120%), 3 repetitions each Recommendation: — For Assay: RSD 2.0% ~ For individal impurity above 0.05%, in general, RSD s10% pay 8 Zi 2023-02-21 5.2.Intermediate precision Expresses variations within laboratories, such as different days, different operators, different equipments, different samples and so forth. * different operators “different instruments “standards and reagents from different suppliers coluntns from different batches *a combination 2023-02-21 5.3, Reproducibility (interlaboratory precision) Expresses the precision between laboratories (collaborative studies usually applied to standardization of methodology). It is considered in case of standardization of the method. Precision + Intermediate precision ~ Test a sample on multiple days, analysts, equipments —RSD should be the same requirement as method precision + Reproducibility (inter-laboratory trial) Not requested in the submission ~Need to be considered for method transfer 2023-02-21 Precision sme Sane Diternt some Dire Dutt sine Same Dire -Muatipte Days Not Specified Soir ii id nearer er meNGn tate ‘Matric design can be used for intermediate precision and reproducibility Random error (precision, represented by STDEV) = total error ~ systemtic error Random error cannot be corrected. Variations in random error can not be predicted. Some sources of random error “Equipment and material “Laboratory (personal, enviroment, etc) “Time “Methods etc 3 2023-02-21 increasing number of random error sources Repontaity| seals 6. The limit of detection (LOD) and Quantification (LOQ) ‘The detection limit isthe injected amount that results ina peak with a height at leat two or three times as high as the baseline noise level LOD =20r3S/N S Lt] iil LOQ=10S/N 2023-02-21 ES SetenceDirect ‘Validation of ehromstogrphic methods: Evasion of detection atid tcton Tints nthe determination of unpuriues i omeprcole tomnoie rt criterion but {fn goalycal systems ut present nofse Tor the base ‘nalytical separation vechniques, such asthe chromatographice, the messirement of mole f ant trivial and often subjective ‘To determine rornolae rao, a comparison ig miade between the sipnals from sample components of ie BLD Concentrations, prepared in the matrix of interest and Chie

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