Siab rhiab heev thiab Ecologically Sustainable Reversed-Phase HPTLC Txoj Kev Rau Kev Txiav Txim Ntawm Hydroquinone hauv Kev Ua Lag Luam Dawb Creams
Mar 20, 2022
Hu rau: ali.ma@wecistanche.com
Mohammed H. Alqarni 1, Prawez Alam 1, Faiyaz Shakeel 2, Ahmed I. Foudah 1 thiab Sultan Alshehri 2,*
Abstract: Hydroquinone(HDQ) yog ib tug natural depigmenting neeg sawv cev, uas yog feem ntau siv nyob rau hauv daim tawv nqaij-toning npaj. Kev nyab xeeb thiab kev nyab xeeb ntawm kev txheeb xyuas ntawm HDQ kom muaj nuj nqis tsis tau txiav txim siab hauv cov ntaub ntawv dhau los. Yog li ntawd, ib qho kev rhiab heev thiab ecologically greener reversed-theem high-performance nyias-txheej chromatography (RP-HPTLC)-raws li kev soj ntsuam tau tsim rau HDQ kwv yees nyob rau hauv plaub yam kev lag luam.ntxuav hniav dawbcream (CWCs). Cov binary ethanol-water(60}:40, v·v−1) sib tov tau siv los ua cov kuab tshuaj ntsuab. Kev kwv yees ntawm HDQ tau ua tiav ntawm 291 nm. Tam sim no RP-HPTLC-based assay yog linear hauv 20–2400 ng band-1 range. Txoj kev ntsuas tam sim no yog qhov muaj txiaj ntsig zoo raws li kev tshawb pom thiab cov ntaub ntawv kom muaj nuj nqis. Lwm qhov validation tsis, xws li raug, precision, thiab robustness, kuj haum rau kev txiav txim ntawm HDQ. Qhov siab tshaj plaws HDQ tau txais hauv CWC A (1.23 feem pua w·w−1) tom qab ntawd CWC C (0.81 feem pua w·w−1), CWC D (0.43 feem pua w·w−1), thiab CWC B (0.37 feem pua w· w-1). Cov qhab nia analyticalGREEnness (AGREE) rau txoj kev ntsuas tam sim no tau kwv yees li 0.91, qhia txog cov yam ntxwv zoo tshaj plaws ntawm RP-HPTLC tam sim no. Cov txiaj ntsig no qhia tias txoj kev tshuaj ntsuam tam sim no yog qhov muaj txiaj ntsig zoo thiab muaj txiaj ntsig zoo rau kev muaj txiaj ntsig ntawm HDQ hauv nws cov qauv kev lag luam.
Ntsiab lus:pom zoo;hydroquinone; ecologically sustainable RP-HPTLC; kev lees paub
Cistanche extracttuaj yeem tshem tawm cov dawb radicals thiab tiv thaiv kev sib sau ntawm tyrosinase.
Nyem rauCistanche cuam tshuam rau whitening
1. Taw qhia
Hydroquinone(HDQ) yog ib tug natural compound, uas muaj nyob rau hauv ob peb daim tawv nqaij-toningcommercial formulations rau kev kho mob ntawm melasma (ib tug kab mob tshwm sim los ntawm over-accumulated ntawm melanin nyob rau hauv tib neeg daim tawv nqaij) [1,2]. Nws yog ib tug muaj zog depigmenting tus neeg saib xyuas thiab yog siv los ua lwm txoj rau tyrosinase [3]. Nws yog ib qho ntawm feem ntau siv tshuaj tua kab mob ntawm tib neeg daim tawv nqaij hyperpigmentation [4,5]. Qhov ua tau zoo ntawm HDQ hauv kev lag luam ntawm daim tawv nqaij-toning formulations txawv ntawm 1.5 mus rau 2.0 feem pua w·w−1[6]. Qhov siab ntawm HDQ (siab dua 5 feem pua w·w−1) ua rau khaus hauv zos thiab leukoderma rau tib neeg daim tawv nqaij [5,6]. Vim nws cov teebmeem tsis sib haum xeeb, ntau lub tebchaws tau txwv HDQ ua ib qhontxuav hniav dawbtus neeg sawv cev ntawm cov tshuaj pleev ib ce [7]. Txawm li cas los xij, ntau qhov kev tshawb fawb soj ntsuam tau qhia ntau yam kev tiv thaiv los ntawmHDQnyob rau hauv kev tswj ntawm txawv skinhyperpigmentary mob xws li melasma, freckles, lentigines, thiab lwm yam. [8,9]. Los ntawm kev xav txog ob qho tib si cov txiaj ntsig thiab kev pheej hmoo ntawm HDQ, nws qhov kev tshuaj xyuas ntau hauv cov khoom lag luam sib txawv ntawm cov tawv nqaij toning yog tsim nyog.
Kev ntsuam xyuas tshuaj sib txawv yog siv rau qhov ntau ntawm HDQ ib leeg lossis ua ke nrog lwm yam.ntxuav hniav dawbCov neeg sawv cev hauv khw muag tshuaj pleev xim dawb (CWCs). Ntau yam ntawm ultra-violet (UV) spectrometry-raws li kev soj ntsuam tau raug sau tseg rau kev txheeb xyuas ntau ntawm HDQ hauv cov khoom lag luam whitening (CWPs) thiab tshuaj npaj [10–13]. Ntau qhov kev ua tau zoo ntawm cov kua chromatography (HPLC)-raws li kev soj ntsuam tau raug sau tseg rau kev txiav txim siab ntawm HDQ nrog rau nws cov ethers hauv ntau hom CWCs thiab CWPs [14–23]. Ntau txoj hauv kev voltametric kuj tau tsim los rau kev txiav txim siab ib txhij ntawm HDQ thiab nws cov ether derivatives hauv CWPs [24–29]. Qee qhov kev tshuaj ntsuam xyuas xws li kev txhaj tshuaj electrochemical [30], micellar electrokinetic chromatography [31], capillary electrochromatography [32], thiab nanocomposite [33] raws li kev soj ntsuam kuj tau tsim los rau covHDQtsom xam nrog rau nws cov derivatives ether thiab lwm yamntxuav hniav dawbcov neeg sawv cev hauv CWPs. Qee cov electrochemical-basednanosensors kuj tau tshaj tawm rau HDQ tsom xam [34,35]. Ib txoj hauv kev zoo-theem-kev ua haujlwm siab-txheej txheem nyias-txheej chromatography (HPTLC)-raws li txoj kev kuj tau siv rau qhov kev soj ntsuam zoo thiab ntau ntawm HDQ hauv CWCs los ntawm peb pawg tshawb fawb [1].
Tom qab kev soj ntsuam tag nrho ntawm cov ntawv tshaj tawm ntawm HDQ tsom xam, nws tau pom tias kev nyab xeeb thiab kev ruaj ntseg ntawm cov tshuaj hauv cov ntaub ntawv tsis tau raug tshuaj xyuas lossis txiav txim siab rau kev ntsuas. Tsis tas li ntawd, cov tshuaj ntsuab/ecologically sustainablereversed-theem HPTLC (RP-HPTLC)-raws li kev ntsuam xyuas tseem tsis tau siv rau kev kwv yees ntawmHDQhauv nws CWCs. Ecologically sustainable/ntsuab HPTLC-raws li kev soj ntsuam muaj ntau yam zoo xws li kev yooj yim, kev lag luam, kev lag luam qis, lub sij hawm luv luv, kev soj ntsuam ntawm ntau cov qauv, nrhiav kom pom tseeb, thiab txo qis hauv ib puag ncig toxicityover HPLC thiab lwm txoj hauv kev analytical [36–39]. Raws li, RP-HPTLC txoj kev rau kev txiav txim siab ntawm HDQ raug xaiv rau txoj kev tshawb no. Cov txheej txheem sib txawv yog siv rau qhov kev ntsuam xyuas ntawm cov ntawv qhia zaub ntsuab ntawm cov kws tshuaj ntsuam xyuas [38–43]. Txawm li cas los xij, tsuas yog analytical GREenness (AGREE) metric mus kom ze siv tag nrho 12 lub hauv paus ntsiab lus ntawm greenanalytical chemistry (GAC) rau kev ntsuam xyuas ntsuab [42].
Qhov pom zoo metric mus kom ze tau siv rau kev ntsuam xyuas ntsuab ntawm txoj kev presentRP-HPTLC [42]. Yog li, txoj haujlwm tam sim no tau ua tiav los tsim kom muaj txiaj ntsig zoo thiab ntsuab / ecologically sustainable RP-HPTLC txoj kev rau kev kwv yees ntawmHDQhauv plaub qhov sib txawv CWCs. Lub greenness profile ntawm tam sim no RP-HPTLC txoj kev tau txais los ntawm AGREE: Lub Ntsuas Greenness Calculator. Qhov kev ntsuam xyuas tam sim no rau HDQ tsom xam tau raug lees paub raws li International Council for Harmonization (ICH) Q2 (R1) cov lus qhia [44].
2. Cov ntaub ntawv thiab cov txheej txheem
2.1. Khoom siv
Tus qauv siv ntawm HDQ (purity: 99 feem pua) tau txais los ntawm Fluka Chemica (Darmstadt, Lub Tebchaws Yelemees). HPLC-qib methanol (MeOH) thiab ethanol (EtOH) tau txais los ntawm Alfa Aesar (Tewksbury, MA, USA). HPLC-qib dej (H2O) tau sau los ntawm Milli-Q dej purifier system (E-Merck, Darmstadt, Lub teb chaws Yelemees). Lwm cov kuab tshuaj andreagents siv tau yog qib analytical. Plaub qhov sib txawv CWCs ntawm HDQ tau txais los ntawm cov khw muag tshuaj hauv Al-Kharj, Saudi Arabia, thaum Lub Rau Hli 2021. CWCs ntawmHDQtau muab khaws cia rau hauv qhov chaw txias thiab tsaus ntawm 22 ◦C ua ntej pib qhov kev sim.Cov CWCs tau khaws cia li ntawm ib hlis ua ntej pib qhov kev sim.
2.2. Chromatography
RP-HPTLC densitometry quantification ntawm HDQ hauv nws cov qauv siv thiab plaub CWC sib txawv tau ua los ntawm HPTLC ntsuas (CAMAG, Muttenz, Switzerland). Kev txheeb xyuas ntau ntawm HDQ tau ua tiav ntawm 10 × 20 cm2 iav-rov qab daim hlau ua ntej coated nrog RP silica gel 60 F254S daim hlau (E-Merck, Darmstadt, Lub teb chaws Yelemees).Cov qauv ntawm TLC daim hlau tau pom raws li 6 hli bands. Kev siv lub tshuab ntsuas tsis siv neeg 4 (ATS4) applicator (CAMAG, Geneva, Switzerland). Tus qauv siv tau haum nrog CAMAG microliter syringe (Hamilton, Bonaduz, Switzerland). Qhov kev thov tus nqi rau qhov kev soj ntsuam ntau ntawmHDQtau khaws cia tsis tu ncua ntawm 150 nL s−1.Cov phaj tau tsim nyob rau hauv ib qho kev loj hlob chamber 2 (CAMAG, Muttenz, Switzerland) ntawm 80 mm nrug. Green solvent system rau HDQ tsom xam yog EtOHH2O (60:40, v·v−1). Lub tsev loj hlob tau saturated yav dhau los nrog cov vapors ntawm lub sijhawm txawb rau 30 min ntawm 22 ◦C. HDQ tau kuaj pom ntawm 291 nm. Qhov ntsuas qhov ntev yog 4 × 0.45 mm2 thiab qhov ntsuas ntsuas yog 20 hli s−1. Txhua qhov kev sim tau ua tiav hauv triplicate. Cov software siv rau kev ua cov ntaub ntawv yog WinCATs (v. 1.4.3.6336, CAMAG, Muttenz, Switzerland).
2.3. HDQ Calibration Curve thiab Kev Npaj Cov Qauv Tswj Xyuas Zoo
Qhov ntau npaum ntawm HDQ (10 mg) tau muab tso rau hauv 100 mL ntawm EtOH-H2O (60: 40, v·v−1) cov kuab tshuaj ntsuab kom ua tiav cov tshuaj hauv Tshuag nrog cov concentration ntawm 100 µg mL−1. Qhov sib txawv ntawm cov kev daws teeb meem tau diluted ntxiv siv EtOH-H2O (60: 40, v·v−1) cov tshuab kom ua tiav HDQ concentrations hauv 20-2400 ng band-1 range. Cov kev daws teeb meem ntawmHDQuas muaj ntau qhov sib txawv tau pom ntawm HPTLC daim hlau. HPTLC thaj chaw siab tshaj plaws rau HDQ tau txais rau txhua qhov HDQ daws qhov kev sim tshuaj tam sim no. Lub calibration nkhaus ntawm HDQ yog generated los ntawm plotting HDQ concentrations tiv thaiv nws HPTLC cheeb tsam. Tsis tas li ntawd, peb qhov sib txawv tswj (QC) cov qauv, xws li qis QC (LQC; 20 ng band-1), nruab nrab QC (MQC; 600 ng band−1), thiab siab QC (HQC; 2400 ng band-1) cov qauv , tau txais nyias nyob rau hauv thiaj li yuav txiav txim siab txawv validation parameters rau tam sim no kws tshuaj ntsuam xyuas.
2.4. Kev ua piv txwv rau kev txiav txim siab HDQ hauv CWCs
HDQ tau muab rho tawm los ntawm plaub qhov sib txawv CWCs los ntawm kev siv cov txheej txheem qhia hauv cov ntaub ntawv [1]. Qhov hnyav hnyav (5.0 g) ntawm plaub CWC sib txawv, suav nrog A, B, C, thiab D, raug xa mus rau qhov sib cais sib cais. Txhua CWCwas shaken nyob rau hauv qhov sib cais funnel nrog MeOH (3 × 70 mL) rau ib lub sij hawm ntawm 30 min ntawm 22 ◦C.Cov MeOH rho tawm los ntawm txhua CWC tau ua ke thiab evaporated nyias mus rau drynessunder txo siab siv lub tshuab nqus tsev evaporator teb. Cov residues tau raug muab rov ua dua nrog 10 mL ntawm MeOH thiab muab cia rau hauv lub tub yees kom txog thaum kev ntsuas ntxiv.Cov qauv tau txais tau raug rau HDQ tsom xam siv txoj kev ntsuas tam sim no ntawm 291 nm.
2.5. Validation Parameters
Tam sim no RP-HPTLC kev ntsuam xyuas rau HDQ tsom xam tau siv tau rau qhov sib txawv validation parameters los ntawm kev ua raws li ICH-Q2 (R1) cov lus qhia [44]. CovHDQlinearity tau soj ntsuam los ntawm plotting HDQ concentrations tiv thaiv nws qhov ntsuas peak cheeb tsam. HDQ linearity raug soj ntsuam ntawm 11 qhov sib txawv QC cov qauv ntawm 20, 40, 60, 100, 200, 300, 400, 500, 600, 1200, thiab 2400 ng band-1 rau tam sim no tshuaj ntsuam xyuas. Qhov system efficiency parameters rau tam sim no analytical txoj kev raug soj ntsuam nyob rau hauv cov nqe lus ntawm retardation factor (Rf), asymmetry factor (As), thiab tus naj npawb ntawm theoretical daim hlau ib 'meter' (N m−1). Cov Rf, As, thiab N m−1 tau txais ntawm MCQ (600 ng band−1), raws li tau tshaj tawm yav dhau los hauv cov ntaub ntawv [45].
Qhov tseeb rau txoj kev RP-HPTLC tam sim no tau txiav txim siab raws li qhov feem pua rov qab.Qhov feem pua rov qab tau txais ntawm LQC (20 ng band−1), MQC (600 ng band−1), thiab HQC (2400 ng band-1) rau txoj kev analytical tam sim no.
Qhov tseeb rau txoj kev tshuaj ntsuam xyuas tam sim no tau raug ntsuas raws li intra/interdayprecision. Intraday precision tau txiav txim los ntawm kev tsom xam ntawm HDQ ntawm LQC, MQC, thiab HQC nyob rau tib hnub rau qhov kev ntsuam xyuas tam sim no. Interday precision tau txiav txim siab los ntawm kev tsom xam ntawm HDQ ntawm LQC, MQC, thiab HQC ntawm peb hnub sib txawv rau kev ntsuas tam sim no [44]. Txhua qhov tseeb tau ntsuas rau lub sijhawm (n=6).
Lub robustness tau soj ntsuam los ntawm kev qhia qee qhov kev hloov me me hauv cov kuab tshuaj ntsuab rau txoj kev RP-HPTLC tam sim no. Rau kev ntsuas kev ua tau zoo, thawj EtOH H2O (60:40, v·v−1) hnyav tau hloov mus rau EtOH-H2O (62:38, v·v−1) thiab EtOHH2O (58:42, v·v−1) ) cov tshuab hnyav, thiab cov lus teb tshwj xeeb HPTLC thiab Rf qhov tseem ceeb raug kaw thiab txhais [44].
Qhov rhiab heev rau txoj kev ntsuas tam sim no tau raug soj ntsuam raws li kev kuaj pom (LOD) thiab ntsuas qhov ntsuas (LOQ) txwv siv tus qauv sib txawv. Lub LOD thiab LOQ ntawm HDQ rau tam sim no analytical method raug xam, raws li qhia nyob rau hauv cov ntaub ntawv [44,45].
Lub ncov purity / tshwj xeeb tau raug soj ntsuam los ntawm kev sib piv Rf qhov tseem ceeb thiab UVspectra ntawm HDQ hauv CWCs A, B, C, thiab D nrog rau cov txheej txheem HDQ rau cov tshuaj ntsuam xyuas tam sim no.
2.6. Quantitative Analysis ntawm HDQ hauv CWCs
Cov qauv tau txais ntawm CWC A, B, C, thiab D tau pom ntawm HPTLC daim hlau, thiab lawv cov lus teb TLC tau sau tseg. Lub ncov cheeb tsam rauHDQhauv CWCs tau sau tseg. Cov HDQ cov ntsiab lus hauv CWCs tau suav nrog kev siv qhov kev ntsuas nkhaus ntawm HDQ rau txoj hauv kev tam sim no.
2.7. Kev ntsuam xyuas Greenness
Cov yam ntxwv ntsuab rau txoj kev ntsuas tam sim no tau txais los ntawm kev siv AGREE metric mus kom ze [42]. Cov qhab nia pom zoo (0.0–1.0) ntawm txoj kev tshuaj ntsuam xyuas tam sim no tau sau tseg siv qhov pom zoo: Lub Tshuab Ntsuas Kev Ntsuas Greenness (version0.5, Gdansk University ntawm Technology, Gdansk, Poland, 2020).
3. Cov txiaj ntsig thiab kev sib tham
3.1. Txoj kev loj hlob
Raws li cov ntaub ntawv analytical txoj kev, nws tau pom tias ecologically sustainable muaj peev xwm / ntsuab RP-HPTLC txoj kev rau kev tsom xam ntawm HDQ nyob rau hauv kev lag luam tshuaj pleev ib ce yog tsis muaj. Yog li ntawd, tam sim no txoj kev tshawb no yog nqa tawm los tsim kom tau sai, rhiab heev, thiab ecologically sustainable. RP-HPTLC txoj kev rau HDQ tsom xam hauv CWCs.
Rau kev txheeb xyuas RP-HPTLC ntawm HDQ, qhov sib txawv ntawm EtOH thiab H2O, suav nrog EtOH-H2O (50:50, v·v−1), EtOH-H2O (60:40, v·v−1), EtOH-H2O (70:30, v·v−1), EtOH H2O (80:20, v·v−1), thiab EtOH-H2O (90:10, v·v–1), tau raug soj ntsuam raws li cov kuab tshuaj ntsuab rau cov kev txhim kho ntawm ib pab pawg ntseeg siab rau HDQ tsom xam. Cov kuab tshuaj tov tau tsim nyob rau hauv chamber saturation tej yam kev mob. Los ntawm cov ntaub ntawv sau tseg, nws tsis pom tias EtOH-H2O (50:50, v·v−1), EtOH-H2O (70:30, v·v−1), EtOH-H2O (80:20, v·v− 1), thiab EtOH-H2O (90:10, v·v-1) cov kuab tshuaj ntsuab sib xyaw muaj cov chromatogram tsis zoo ntawmHDQnrog rau qhov tsis lees txais As tus nqi (Raws li {{0}}.29). Txawm li cas los xij, EtOH-H2O (60: 40, v·v-1) cov kuab tshuaj ntsuab ua ke tau pom tias muaj kev daws teeb meem zoo chromatogram ntawm HDQ atRf=0.83 ± 0.02 nrog qhov pom zoo Raws li tus nqi (Raws li {{ 12}}.03) (Daim duab 1). Yog li, EtOH H2O (60:40, v·v-1) tau ua kom zoo dua li cov kuab tshuaj ntsuab sib xyaw rau HDQ tsom xam hauv CWCs. UV-spectral bands rau tam sim no RP-HPTLC txoj kev tau kaw densitometrically, thiab qhov siab tshaj plaws HPTLC teb tau pom ntawm 291 nm rau txoj kev presentRP-HPTLC. Yog li ntawd, tag nrho cov kev ntsuam xyuas ntawm HDQ tau ua ntawm 291 nm.
3.2. Validation Parameters
Tam sim no cov kws tshuaj ntsuam xyuas rau HDQ kom muaj nuj nqis tau raug lees paub rau cov kab sib txawv, cov kab ke ua haujlwm tsis zoo, qhov tseeb, qhov tseeb, qhov muaj zog, rhiab heev, thiab qhov siab tshaj plaws purity / tshwj xeeb los ntawm kev ua raws li ICH cov lus pom zoo [44]. Cov txiaj ntsig rau qhov tsawg tshaj plaws-squares regression tsom xam ntawm calibration nkhaus ntawm HDQ rau RP-HPTLC txoj kev tam sim no tau nthuav tawm hauv Table 1.HDQcalibration nkhaus yog linear nyob rau hauv thaj tsam ntawm 20-2400 ng band nrog kev txiav txim coefficient ntawm 0.9997 rau txoj kev ntsuas tam sim no. cov ntaub ntawv no tau pom zoo linearity ntawm HDQ concentration thiab nws cov lus teb.
Cov txheej txheem kev ua tau zoo ntawm txoj kev siv tshuaj tam sim no tau kawm ntawm MQC (600 ng band−1), thiab cov txiaj ntsig tau suav nrog hauv Table 2. Cov Rf, As, thiab N m−1values rau txoj kev ntsuas tam sim no tau kwv yees li 0.83 ± 0.02, 1.03 ± 0.03, thiab 4987 ± 2.87, feem. Cov txiaj ntsig no tau qhia tias txoj kev ntsuas tam sim no muaj kev ntseeg siab rau HDQ tsom xam hauv CWCs.
Cov txiaj ntsig rau kev txheeb xyuas qhov tseeb rau txoj kev ntsuas tam sim no tau teev tseg hauv kab lus 3. Qhov feem pua rov qab ntawm HDQ rau RP-HPTLC txoj kev tam sim no tau txiav txim siab li 101.80 feem pua, 98.16 feem pua, thiab 99.38 feem pua ntawm LQC, MQC, thiab HQC, raws li. . Cov txiaj ntsig siab ntawm feem pua ntawm cov nyiaj rov qab tau qhia qhov tseeb ntawm txoj kev RP-HPTLC tam sim no rau HDQ tsom xam hauv CWCs.
Qhov tseeb tau txiav txim siab raws li qhov feem pua ntawm cov coefficient ntawm kev hloov pauv (feem pua CV), thiab cov txiaj ntsig tau qhia hauv Table 4. Qhov feem pua CVs ntawm HDQ rau txoj kev ntsuas tam sim no tau kwv yees li 0.91, 0. 59, thiab 0.26 feem pua ntawm LQC, MQC, thiab HQC, raws li, rau qhov intradayprecision. Cov feem pua CVs ntawm HDQ rau RP-HPTLC txoj kev tam sim no tau kwv yees li 0.98, {{10}}.69, thiab 0.32 feem pua ntawm LQC, MQC thiab HQC, feem, rau interday precision. Tus nqi qis ntawm feem pua CV qhia qhov tseeb ntawm tam sim no RP-HPTLC txoj kev rau HDQ tsom xam hauv CWCs.
Cov txiaj ntsig ntawm kev txheeb xyuas qhov ua tau zoo rau txoj kev ntsuas tam sim no tau pom nyob rau hauv Daim duab 5. Qhov feem pua CVs rau kev txheeb xyuas qhov muaj zog tau kwv yees li 0.59–0.66 feem pua rau cov txheej txheem presentanalytical. Rf qhov tseem ceeb ntawm HDQ tau pom nyob rau hauv 0.82–{7}}.84 ntau yam rau cov txheej txheem tam sim no. Qhov kev hloov pauv nqaim hauv Rf qhov tseem ceeb ntawm HDQ thiab qis feem pua CVs qhia qhov muaj zog ntawm txoj kev ntsuas tam sim no rau HDQ kom muaj nuj nqis hauv CWCs.
Qhov rhiab heev rau txoj kev ntsuas tam sim no tau sau tseg tias "LOD thiab LOQ", thiab lawv cov txiaj ntsig ntawm lub cev tau qhia hauv Table 1. "LOD thiab LOQ" rau cov txheej txheem tam sim no tau kwv yees li 6.91 ± 0.23 thiab 2. 0.73 ± 0.68 ng band-1, ntsig txog, rauHDQkom muaj nuj nqis. Cov txiaj ntsig ntawm lub cev ntawm "LOD thiab LOQ" rau txoj kev tshuaj ntsuam xyuas tam sim no qhia qhov kev xav tau rau HDQ tsom xam hauv CWCs.
Lub ncov purity / tshwj xeeb rau txoj kev ntsuas tam sim no tau soj ntsuam los ntawm kev sib piv cov overlaid UV spectra ntawm HDQ hauv plaub CWCs sib txawv nrog cov qauv HDQ. Lub overlaid UV spectra ntawm tus qauv HDQ thiab HDQ nyob rau hauv plaub qhov sib txawv CWCs muaj nyob rau hauv daim duab 2. Qhov siab tshaj chromatographic teb rau HDQ nyob rau hauv standard HDQ thiab kawm CWCs tau soj ntsuam ntawm 291 nm rau tam sim no analytical txoj kev. Qhov zoo tib yamUV spectra, Rf qhov tseem ceeb, thiab wavelength ntawm HDQ nyob rau hauv tus qauv HDQ thiab CWCs qhia lub ncov purity / tshwj xeeb rau tam sim no analytical txoj kev.
3.3. Kev soj ntsuam ntawm HDQ Cov Ntsiab Lus hauv CWCs
Kev siv tau ntawm qhov kev tshuaj ntsuam xyuas tam sim no tau txheeb xyuas hauv qhov kev kwv yees ntau ntawm HDQ hauv CWCs. Lub chromatogram ntawmHDQlos ntawm CWCs tau txheeb xyuas los ntawm kev sib piv nws TLC qhov chaw ntawm Rf {{0}}.83 ± 0.02 nrog cov qauv HDQ rau txoj kev ntsuas tam sim no. Cov chromatograms ntawm HDQ nyob rau hauv CWCs A thiab B rau qhov tam sim no analytical assay yog summarized nyob rau hauv daim duab 3. HPTLC chromatograms ntawm HDQ nyob rau hauv CWCs yog zoo tib yam rau cov ntshiab HDQ. Qee lub ncov ntxiv kuj tau tshwm sim hauv chromatograms ntawm CWCs, uas tej zaum yuav cuam tshuam nrog cov excipients sib txawv hauv CWCs. Txoj kev ecologically sustainable HPTLC yog xaiv rau HDQ tsom xam ntawm Rf=0.83 yam tsis muaj kev cuam tshuam los ntawm lwm cov khoom xyaw ntawm CWCs. Tus nqi Rf (0.83) ntawm HDQ hauv CWCs tau pom tias zoo ib yam nrog cov qauv HDQ ({{20}}.83), qhia tias tsis muaj kev cuam tshuam ntawm HDQ thiab CWC cov khoom xyaw. Li no, tsis muaj kev cuam tshuam ntawm kev tsim cov khoom xyaw ntawm qhov zoo ntawm HDQ chromatogram, LOD, thiab kev ua haujlwm ntawm HPTLC txoj kev tshawb xyuas HDQ tam sim no. Lub xub ntiag ntawm cov peaks ntxiv nyob rau hauv chromatograms ntawm CWCs qhia tias tam sim no RP-HPTLC txoj kev ntseeg tau rau HDQ kwv yees nyob rau hauv muaj cov khoom xyaw formulation. Cov ntsiab lus HDQ ntawm CWCswere txiav txim siab los ntawm qhov kev ntsuas nkhaus ntawm HDQ, thiab cov txiaj ntsig tau suav nrog hauv Table 6.Table 6 kuj tseem sau cov ntawv sau npe ntawm HDQ thiab nws cov khoom xyaw tsim. Cov ntsiab lus HDQ tau siab tshaj hauv CWC A (1.23 feem pua w·w−1) tom qab los ntawm CWC C (0.81 feem pua w·w−1), CWC D (0.43 feem pua w·w −1), thiab CWC B (0.37 feem pua w·w−1). Cov ntaub ntawv kaw tseg ntawm HDQ tau qis dua tus nqi sau npe (2.00 feem pua w·w−1) ntawm HDQ hauv CWCs kawm. Cov HDQ cov ntsiab lus hauv ob qhov sib txawv CWCs (A thiab B) tau sau tseg li 0.69 feem pua w·w−1 thiab 0.34 feem pua w·w−1, raws li, siv cov txheej txheem HPTLC ib txwm nyob hauv cov ntaub ntawv [1]. Cov ntsiab lus tshaj tawm ntawm HDQ kuj tseem qis dua li cov ntawv sau npe (2.00 feem pua w·w−1) ntawm HDQ hauv cov ntaub ntawv [1]. Ob peb CWCs lossis CWPs tau ua lag luam raws li kev lees paub tias yog txhua yam-natural.Txawm li cas los xij, nws yog ib qho uas yuav pom qee cov tshuaj hluavtaws xws li deev luag poj luag txiv nrog cov txiaj ntsig zoo sib xws hauv CWCs lossis CWPs li kev dag ntxias. Tus nqi ntawm HDQ tau sau tseg hauv qhov haujlwm no thiab cov uas tau sau tseg hauv cov ntaub ntawv tau qhia tias CWCs tau kawm muaj qhov tsawg ntawm HDQ thiab tsis phim daim ntawv thov [1]. Li no, nws yuav tsum tau kawm CWCs muaj qee cov tshuaj hluavtaws ua neeg deev luag poj luag txiv. Zuag qhia tag nrho, tam sim no analytical assay tuaj yeem siv rau HDQ tsom xam hauv kev npaj tshuaj pleev ib ce thiab tshuaj.
3.4. Kev ntsuam xyuas Greenness
Cov txheej txheem sib txawv yog siv rau kev ntsuam xyuas qhov ntsuab ntawm cov kws tshuaj ntsuam xyuas [38–43]. Txawm li cas los xij, tsuas yog AGREE txoj hauv kev siv tag nrho 12 lub hauv paus ntsiab lus ntawm GAC rau kev ntsuam xyuas ntawm ntsuab [42]. Yog li ntawd, qhov greenness profile ntawm tam sim no analytical method tau txais siv lub AGREE Calculator. Cov qhab-nees AGREE tau kwv yees siv 12 lub hauv paus sib txawv ntawm GAC rau qhov kev tshuaj ntsuam xyuas tam sim no tau nthuav tawm hauv daim duab 4. TheAGREE cov qhab nia rau cov ntsiab lus sib txawv ntawm GAC tau sau tseg raws li hauv qab no: Cov qauv kev kho mob: 0.61Txoj haujlwm ntawm cov cuab yeej tshuaj ntsuam xyuas: 1.{{ 9}}Cov kauj ruam rau kev npaj ua piv txwv: 1.00Degree of automation: 0.80Derivatization: 1.00Cov khoom pov tseg: 1.{{17} }Kev soj ntsuam dhau los: 1.00Kev siv hluav taws xob: 1.00Simple kho: 0.51Source of reagent: 1.00Toxicity of solvents: 1.00 Tus neeg teb xov tooj kev nyab xeeb: 1. 00
Tag nrho cov qhab nia AGREE rau txoj kev tshuaj ntsuam xyuas tam sim no tau sau tseg ua 0.91, qhia txog txoj kev tshuaj ntsuam ntsuab zoo heev rauHDQkom muaj nuj nqis.
4. Cov lus xaus
Txoj kev RP-HPTLC-densitometry yog tsim los rau HDQ tsom xam hauv plaub CWC sib txawv ntawm HDQ. Qhov kev ntsuam xyuas RP-HPTLC tam sim no tau raug lees paub rau qhov sib txawv validation parameters. Txoj kev tshuaj ntsuam xyuas tam sim no yog qhov rhiab heev, nrawm, thiab ecologicallysustainable rauHDQtsom xam. Qhov qhab nia AGREE rau txoj kev ntsuas tam sim no qhia txog kev ntsuas kev ntsuas zoo rau HDQ kom muaj nuj nqis. Tam sim no RP-HPTLC txoj kev yog tsim nyog rau HDQ tsom xam nyob rau hauv plaub txawv CWCs. Cov txiaj ntsig no tau qhia tias tam sim no kev tshuaj ntsuam xyuas tuaj yeem siv rau HDQ tsom xam hauv kev npaj tshuaj pleev ib ce thiab tshuaj sib txawv.
