Kev kuaj pom ntawm 15 ARCRodyn tshuaj tsis raug cai ntxiv rau kev sib deev-txhim kho cov khoom ntawm HPLC-MS / MS nrog cov khoom siv nuclarnel cov chromatographic kem

Abstract:

Lub Hom Phiaj los tsim kho HPLC-MS / MS txoj kev nrog cov khoom siv nuclarle chromatogromoic chromatographic kem los txiav txim cai 15 yam khoom tsis raug cai ntxiv rau kev sib deev-txhim kho cov khoom. Cov hau kev kev tsom xam tau ua los ntawm HPLC-MS / MS system, nrog cunecs-c18 (15 0 hli × 4.7 μm) kem. Ntau cov tshuaj tiv thaiv (MRM) tau ua los txheeb xyuas thiab ntsuas cov khoom siv, cov neeg siv nyiaj, Pseudetafil, Stanozolol thiab Danazol, uas tau muab rho tawm nrog Methanol los ntawm Ultrasonic. Cov txiaj ntsig tau qhia txog kev sib cais ntawm 15 lub tshuab siv tshuaj tiv thaiv ntawm R 2 ntau dua lossis sib cais nrog kev sib cais zoo dua thiab cov kab sib cais zoo dua. Qhov precision ntawm cov txheej txheem tau qhia los ntawm RSD (n {16}}}) los ntawm rau tus nqi kwv yees li ntawm {25% rau 3.3%. Tus nqi rov qab tau txiav txim siab ntawm peb qhov kev ntxiv yog los ntawm 88.3% rau 1 {29% thiab RSD yog los ntawm {}. 9% rau 5.2%. Qhov ntau ntawm kev txwv ntawm kev txwv (LoQ) tau los ntawm {{}}}}}}}}}}}}}}}}}}}}}}}}}}}}} Nees nkaum ntawm cov qauv zoo ntawm 25 cov khoom lag luam-txhim kho cov khoom tau kuaj pom kom ntxiv nrog Sildenafil thiab nrog tus nqi tsis tsim nyog ntawm 80%. Xaus Cov qauv yog qhov tshwj xeeb thiab tau yooj yim los ntes tau 15 Aidodyn tshuaj tau ntxiv tsis raug cai ua ke hauv kev sib deev-txhim kho cov khoom lag luam. Nyob rau tib lub sijhawm, tus nqi kom zoo kom tau txais kev pom zoo, thiab cov cai tswjfwm yuav tsum tau muab cov cai tswj hwm kev noj qab haus huv thiab kev nyab xeeb ntawm cov neeg.

 

Lo lus tseem ceeb: khoom nuclear particle chomatogromaphic kem; HPLC-MS / MS; Sex-txhim deev khoom; Afododyn; ntxiv tsis raug cai; PhyLolamine Mesylate; Noracetildenafil; acetildenaf; vardgalafil; sildenafil; hydroxyhomosildenaf; Homosildenaf; Aminotadalafil; tadalafil; Thioaildenaf; pseudovgenafil; norneosenfil; methyltestosterone; stanolol; danazol

 

100% ntuj tshuaj ntsuab cistance cov khoom pab rau txhim kho kev sib deev hauv kev kho mob ntev

 

 

Nyob rau hauv xyoo tsis ntev los no, qee cov neeg ua txhaum cai siv tshuaj lom neeg ntxiv rau cov zaub mov noj qab haus huv, thiab cov neeg siv khoom tsis zoo los ntawm kev txhawb nqa cov haujlwm thiab cov khoom siv ntawm cov khoom lag luam. Hom rooj plaub no tseem hu ua qhov thiaj li hu ua cov tshuaj tsis yog tshuaj tsis zoo ntawm cov tshuaj siv tshuaj. Xyoo tsis ntev los no, cov khoom lag luam feem ntau muaj kev koom tes nrog cov "hu ua" kev sib deev khoom noj ".
Cov khoom lag luam kev sib deev no tau tawm hauv kev ua lag luam nyob rau hauv ib tug kawg ntws, feem ntau yog muag online thiab hauv xov tooj. Lawv cov yam ntxwv yog lawv cov khoom ntim khoom thiab cov khoom lag luam muaj cov ntaub ntawv pom tseeb, xws li "Kev cog qoob loo ntawm kev ua rog", "
Cov khoom no tau thov kom tsis muaj kev phiv los thiab muaj zog, tab sis qhov tseeb, lawv ntxiv aphrodisiac tshuaj lom neeg cov tshuaj. Kev noj cov khoom noj kev noj tshuaj lom neeg uas tsis raug cai ntxiv cov tshuaj xyaw tshuaj no tuaj yeem ua rau lub zeem muag, kiv cua, thiab npog cov tshwm sim ntawm cov kab mob plawv. Thaum muaj mob hnyav, nws tuaj yeem ua rau ntshav siab lossis tuag tam sim ntawd, uas mob siab rau tib neeg kev noj qab haus huv [1-2]. Nyob rau hauv xyoo tsis ntev los no, muaj ntau cov lus ceeb toom kev txiav txim siab ntawm kev tsis raug cai rau cov zaub mov noj qab haus huv thiab cov tshuaj Suav pentins [2-17]. Cov tub ntxhais cov khoom siv chromatographe chromatography yog qhov ua rau cov chromatographic tshiab tsim thev naus laus zis tsim tawm hauv xyoo tsis ntev los no. Thi Technology Ua kom zoo rau kev ua haujlwm rov qab siab ntawm kev ua kom muaj kev sib cais ua kua chromoography, thiab ua kom muaj peev xwm ua kua rau ultra-siab, thiab muaj ntau yam thiab nrov. Hauv qhov kev sim no, cov tub ntxhais cov tub ntxhais chromatograph tau thov rau heplc-ms / ms los ua ib txhij thiab nrawm 15 aphrodisiac siv tshuaj rau kev saib xyuas kev noj qab haus huv.

 

1 cov ntaub ntawv thiab cov hau kev

1.1 seev

Kev ua kom zoo ua kua chromatography-Tandem Quadromole ntau spectromograph, agent 6410 tandem quadrupter, allent, Asmeskas; Mili-u deion tshuab dej, millipore, USA.

1.2 kuaj thiab reagents
Tag nrho ntawm 25 cov kev sib tw ntawm cov khoom siv kho mob sib deev tau ntsuas hauv kev sim, txhua yam uas tau kuaj xyuas los ntawm Hangzhou Kev Saib Xyuas Kev Lag Luam thiab Cov Thawj Tswj Xyuas Kev Lag Luam thiab Chaw Tswj Xyuas Kev Lag Luam. Kev siv tshuaj physolamine mesylate mesylate (batch} {}}}, loj}, thiab danazol (batch tooj {}} 99.3%) tau yuav los ntawm Tuam Tshoj Cov Khoom Noj Khoom Haus thiab Tshuaj Yeeb Tshuaj. Redenafil (batch tooj 1591-080 A3, pawg feem {}} A1 {16} {}} A1, pawg feem 99.3%) tau yuav los ntawm Tuam Tshoj Cov Khoom Noj Khoom Haus thiab Tshuaj Yeeb Tshuaj. 100%), HydroxyhomosildFilil) {29%), KAWG {} A2, KAWG {3.7%), Tadalafil (Batch tus lej 1156-051 A1, pawg feem 99.5%), pass {} {} {54}} A2, pawg feem 99.9%) tau yuav los ntawm TLC Cov Qauv Tshuaj, Canada. Formic acid tau tsom xam qib thiab methanol yog chromatographic qib.

 

1.3 Chromatographic mob

Cov Chromatterraphic kem yog cortecs-c18 (15 0 hli × 4.6 hli, 2.7 μm); Cov mobile theem yog 0.1% formic acid aqueous daws-methanol, thiab cov gradient Kaus Txoj Kev Kawm yog: {} {{% Methanol; {{13 {13}} Min, 90% {15}}} Methanol; 20-25 Min, 100% {-50 Methanol;
Kab ntsuas kub 4 0 degree; Ntim Flow tus nqi 0.3 ml / min; Txhaj ntim ntim 10 μl.

 

1.4 Pawg Tshaj Tawm Ntau Yam

Iion Source: Electrospray Ion qhov (ESI), muaj txiaj ntsig ion Nrhiav tau hom (esi +); Ntau cov tshuaj tiv thaiv kev tshuaj xyuas (MRM hom); scanning nrog segmented mrm hom; kom qhuav roj kub 350 degree; Cov roj kom qhuav roj yeeb Flow 10 l / min; Nebulizen siab 200 kpa; capillary voltage 4 kv; Kev ntsuas hluav taws xob: pawg Axis tsis siv neeg; Lwm cov khoom siv huab hwm coj ntawm kev soj ntsuam ntau ntawm 15 Aphrodisiac cov khoom siv muaj cov ncauj lus kom ntxaws hauv lub rooj 1.

 

1.5 Npaj Txog Kev Siv

Qhov ntsuas hnyav txog 1 {{{{mg ntawm txhua ntawm ib qho ntawm 15 ml volumetric cov kev daws teeb meem ntawm txog {mg / ml txhua. Pipette Pipette 0.}}}}}}}}}}}}}}.}.}}}.}}.}}.}

1.6 Npaj txoj kev ntsuas ntsuas
Siv 1 g ntawm cov khoom no, tso nws hauv ib qho 5 0 mlthanol, ntxiv rau 256 KHz), txias, thiab dilute rau teev nrog mobile theem. Lim nrog 0.2 μm lim mem tes. Txij li thaum muaj cov khoom siv ntawm cov khoom siv tau zoo ntxiv, cov qauv kev sib deev tuaj yeem tsim nyog tau nce los yog cov qauv kev sib deev muaj peev xwm ua kom nws qhov kev pom zoo nyob rau hauv cov kab.

100% ntuj tshuaj ntsuab cistance cov khoom pab rau txhim kho kev sib deev hauv kev kho mob ntev

2 cov txiaj ntsig

2.1 cov txiaj ntsig chromatographic tau

Siv sijhawm 15 npaj siv cov tshuaj sib xyaw ua ke, txhaj rau 5 μl, thiab cais lawv cov tub ntxhais me me logbromelco C18 (150 hli × 4.6 hli, 2.7 μm). Cov txiaj ntsig tau pom hauv daim duab 1. Nws tuaj yeem pom tau tias peb lub Chromatographic Peaks ntawm Sildenafil, Hydroundenafil thiab yog tib lub sijhawm khaws cia. Nyob rau tib lub sijhawm, kev tuav lub sijhawm ntawm Pseudovardenfardenfardafil thiab Narmosildenafil kuj tseem zoo ib yam. Qhov kev sim no siv ib qho qauv uas nrog tib lub loj uas muaj kev sib xyaw ua cov tshuaj sib xyaw ua ke kom paub tseeb. Cov txiaj ntsig qhia tau hais tias ntau cov khoom siv nrog lub sijhawm sib npaug zoo sib xws tsis muaj kev sib tw inhibition rau ib leeg.

Cov lus 1 ms tsis rau 15 ARCRodyn yeeb tshuaj

 

Ib feem	Ntsuas m / z (m / z)	Ionization zog / V	Ionization muaj peev xwm (ev)
-Pinene	120	120	9.39
Limonene	120	120	9.26
-Caryophellophes	130	130	9.56
Myrcene	100	100	9.12
D-limonene	100	100	9.22
Terpinolene	120	120	9.34
-UaCulene	130	130	9.47
-Terpinene	120	120	9.20
-Pinene	130	130	9.45
-Terpineol	120	120	9.39

 

2.2 linear kev tshawb nrhiav kev tshawb nrhiav, nrhiav kom muaj kev txwv thiab quantative txwv

Nqa 5 μl ntawm cov npaj siv cov lus qhia txog kev daws teeb meem, thiab siv cov khoom noj ntawm cov khoom siv Abscissa (X) los tshuaj xyuas cov kab kev sib raug zoo. Cov txiaj ntsig tau tshwm sim hauv rooj 2.
Siv 1 g ntawm cov qauv khoob (hnub ci hluav taws kub cov tshuaj tiv thaiv kab mob, thiab kom tau txais cov kev ntsuas tsis raug cai thaum muaj 3 thiab 10, feem. Cov txiaj ntsig tau tshwm sim hauv rooj 2.

100% ntuj tshuaj ntsuab cistance cov khoom pab rau txhim kho kev sib deev hauv kev kho mob ntev

 

2.3 Cov qauv kev ntsuas ruaj khov

Nqus tawm 1 g ntawm cov qauv seem (Sunshine tus txiv neej tua hluav taws fais fab, thiab ua kom muaj kev ntsuas ntawm kev sib xyaw ntawm kev ntsuas ntsuas 8 tus txiv neej / ml / mL. RSD ntawm lub ncov thaj tsam ntawm 5 rov qab txhaj hauv 1 hnub yog coj los ua qhov kev txhaj tshuaj (3 rov ua dua tshiab Cov txiaj ntsig tau tshwm sim hauv rooj 2.