China_phthalate_solution

DBEP
17.8 9 4 ਪ Э ‫ࡑل‬ෝ‫ل‬༂ ᴈ
DPP
18.013 ਪЭ‫ࡑل‬ෝ‫࠴ߓ ل‬ᴈ
DCHP
19. 416 ਪ Э ‫ ࡑ ل‬ෝ‫ل‬Ɠ4 -ࡑ ࠕ -2༂ ࠕƔᴈ D M P P
19.929 ਪЭ‫ࡑل‬ෝ‫࠴ل‬ᴈ
DHXP
22 .6 4 4 ਪ Э ‫ ࡑ ل‬ෝ‫ل‬Ɠ2-ၠ ࠕƔ࠴ ᴈ
24
18
ऱजऔǖUPLC/PDAऱज A.UPLC/PDA ᄟୈ
ၕఝ༩๫ƥ ೫௽ᇿƥ ѶӐƥ ᇿ໘ƥ ੇ෕ƥ ੇ‫׵‬པƥ
Waters UPLC H-Class/PDA ACQUITY UPLC HSS C18 (1.7um, 2.1×100mm) 225nm 45˚C 0.4mL/min A-ඪƗB-ၠᦝƗ࣐ྡྷื؎༨ຉ
B. MSᄟୈ: ༩๫ƥ ACQUITY UPLC TQD ঢ়ሷߋ଍൛ƥ ESI+ ‫׏‬ঢ়‫׏‬࿩ƥ 3.2KV ঢ়ሷჾ໘؎ƥ 120˚C ຉಾ࠻ఞ໘؎ƥ400˚C ຉಾ࠻ఞੇਏ"650L/Hr
๴ 2.ACQUITY UPLC TQDè
18ᇜਪЭ‫ࡑل‬ෝ࿾‫ٺ‬༌ࢹ‫ݛ‬୰؎ƥ10ppbƓDMPçDMEPçDEEPçDEPç DPhPçDEHPçBBPçDIBPçDBPçDBEPçDPPçDCHPçBMPPçDHXPçDNOPçDINPç DNPçDIDPƔè
DEHP
23.103 ਪ Э ‫ࡑل‬ෝ‫ ل‬ᆥྒྷ ᴈ
DNOP
23.727 ਪЭ‫ࡑل‬ෝ‫ل‬ၺಫᴈ
DINP
24.335 ਪЭ‫ࡑل‬ෝ‫ل‬ಫᴈ
DNP
24.570 ਪЭ‫ࡑل‬ෝ‫ل‬ၺ‫ݏ‬ᴈ
DIDP
ख़ ኔ೰
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
ऱजጙǖUPLC/MS/MSऱज ဣዩᄟୈ
A. UPLCᄟୈ:
LC༩๫ƥ
ACQUITY UPLC H Class༩๫
೫௽ᇿƥ ੇ‫׵‬པAƥ
ACQUITY UPLC HSS C18,1.7μm,2.1X100mmƗ 0.1%FAඪಾ၈
ੇ‫׵‬པBƥ
ၠᦝ
ੇ෕ƥ
0.4ml/min
ื؎༨ຉ" ื؎ѝ
ಪ ఝ Г ᆪਛ ໞ ‫ ֬ ׮‬ಪ ཹ ୆ Ʀ೫௽ ᇿ ܼ য় ఝ ฻ ‫܉‬ਛ‫ ئ‬౼ პ ֬ ਹࠊྦƗ໘؎ٚຽເ4ᇇ90 °CƗѰढ़‫ࡍצ‬ൗႯè
ൺ६֬ᇓ੄฿࠙ƥACQUITY UPLC H-Class֬SmartStart࠶ඓƓሌ৭ և ூƔढ़๤ ൏ ‫ ؎ื ؚ‬ఖ ൚ ൏ ࡞ ‫ ދ‬۹ ۸ ხ ሆ ത ҋ ᇮ ࣐ ྡྷሸ‫׵‬ ܼ য় è๠ ‫ ࢃ ݝ‬ᆊ ཻ‫ ৼ ֬ ྟ ׌‬࿊ ‫ ݝ‬Ӹ ‫ ࡍ צ‬ఖ দ Ɨ୆ ‫ ܛ‬ቒ ս Ӹ ؎‫׀‬෱ؒ࿝ߓ൏࡞è
ਪЭ‫ࡑل‬ෝ‫ل‬2-‫ק‬ဥࠕၠᴈDBEPç ਪЭ‫ࡑل‬ෝ‫ل‬4-ࡑࠕ-2-༂ࠕᴈBMPP
Ю١ٌࣁജਛ਍ᇜࠕ჆໬า൞Әۡཹ၈པ೫௽࠶ඓƓUPLC ࠶ඓƔ‫ٺ‬༌18ᇜƓ‫ݪ‬ขຝFDAး౷ƔਪЭ‫ࡑل‬ෝ࿾֬١ٌƗ١ ٌ၉ເҗႯ໬า൞Әۡཹ၈པ೫௽ᇐ௽৺Ⴏ࠶ඓƓUPLC/MS/ MSƔƗ‫ۅ‬١ٌकႼ‫ٺ‬༌෕؎ঀƗਹ଀؎ۡ֬า‫׋‬è൨Ⴏ჆൓ မ൰ႡႼᇐ௽༩๫Ѱማ౷ࡦҰਹ଀؎֬Ⴏ߃è١ٌ‫ل‬ເҗ Ⴏ໬า൞Әۡཹ၈པ೫௽༩๫‫ܼࠥلދ‬ᆛਠࡦҰఝƓUPLC/ PDAƔ‫ٺ‬༌١ٌƗ൨Ⴏ჆ᄧ൏ߕ҉कႼᇐ௽༩๫֬Ⴏ߃è
\።፿ଗገ^
ज़໦ĐᏠđ፻
——ᆼᄂီ18ᒬ೺‫۽‬औଡႭዎUPLC/MS/MSॊᇜஊ௼ऱ‫ښ‬
ࣔಷƗขຝૉ฿И֨ਛఖᄐ࠻ᄬൺᅀෘ࠻໱ಠ֬ൠࡸƗ֤ᇈ ൑௝τ಍ࡦҰ൮Ӎ‫؟‬൏‫ڋ‬ఖõᄐöႫƗਪЭ‫ࡑل‬ෝ࿾֬ࡦҰ ᄣ؎ӵເಭ૓ܸሆ֬࢑‫׋‬è
ఖᄐ࠻ƓჂଇࠇራ࠻çೋራ࠻çᅀራ࠻Ɣ၀ः൥໨૓ӏන֬ ೋߋໞ‫࠻׮‬èᇽး႒Ⴏ჆ႉਟ‫ދ‬ଶ৒ᇌ௝èᄤႉਟᇖൗႯƗ Ⴜሀ჆൫٩თГ੄‫ݛ‬ᆳႉਟ֬བྷఞƗЎટ‫ݛ‬ᆳႉਟ֬ၺ໌ç ᄝ໌Ɨ၀୆ᅀృ‫ݛ‬ᆳႉਟ८‫֬ے‬ೕ߈ྦçޯ൓‫ے‬ƗႴఊ൥Ⴜ ཹ‫ۆ‬਌‫ݛ‬ᆳႉਟ֬ๆಝ‫ܻے‬Ɨ཈ᇾ฻ۡ‫ݛ‬ᆳႉਟ֬௝ᇐᇐ ਏèఖᄐ࠻֬ᇽးӵ‫ٺ‬ເ‫໌ڋ‬Ⴙç֍฿བྷႹçᅀᇞ࠻çೋߋ ໞ‫࠻׮‬çೋߋ࠻çඪƗ෸Юഭ‫ؚ‬ಭ฿ѰેႼູ‫ݤ‬ƗЮ՘ൠࡸ֬ ‫ن‬ഺ൥Ⴕ჆ങඛఖᄐ࠻ഺӈӓࡌເࢍֵӵЮൗႯᄤ൑௝ᇖ ࣓Ⴏ֬ᅀෘ࠻৒༅ᇐਪЭ‫ࡑل‬ෝ࿾քเჷЮ႒‫ۅ‬ൗႯ֬ሼ ᢰႹƗ՝‫ؾ‬ႋ‫ن‬ਛ൑௝τ಍ൠࡸè
18ᇜਪЭ‫ࡑل‬ෝ࿾೫௽‫ٺ‬༌ࢹ‫ݛ‬೉༶๴෵൜
ۣഔဟମ )min*
ᒦᆪ෗߂
፞ᆪ ෗߂
4.482 ਪЭ‫ࡑل‬ෝ‫ࡑل‬ᴈ
DMP
4 . 8 9 6 ਪ Э ‫ ࡑ ل‬ෝ‫ل‬Ɠ2-ࡑ ဥ ࠕƔၠ ᴈ
DMEP
8.483 ਪЭ‫ࡑل‬ෝ‫ل‬ၠᴈ
DEP
8 .6 22 ਪ Э ‫ ࡑ ل‬ෝ‫ل‬Ɠ2-ၠဥ ࠕƔၠ ᴈ
ਈ᎖Waters ACQUITY UPLC TQD
໬า൞TQࡦҰఝ൥ເ၉฿ߋ֬UPLC®/MS/MS‫׮‬ਏ‫ٺ‬༌‫ؾ‬ा‫ن‬ ֬ၕఝƗչ֥Ը৺වࠥ‫ۍ‬MS֬ቒࡋ࿑ᄻྦçໞ‫ྦ׮‬ç෕؎ ࠪሠಙྦèເఛ‫ލ‬UltraPerformance LC®UPLC֬Әۡྦ୆ƗTQ ࡦҰఝၢቒঀ֬෕؎җࠩඛओèთACQUITY UPLC®༩๫၉๤ ൗႯƗACQUITY® TQD ༩๫ເႯ߃෵Ⴜ֬‫׮‬ਏ‫ٺ‬༌฻‫༼਼܉‬ ֬‫ٺ‬༌ࡦҰདྷ‫ٺ‬і੸ࠪဩ௝๠ਏƗ႒ႯٚຽЎচƥഺ༅‫ٺ‬ ༌çADME೸࿑ç൑௝τ಍çߓࣩ࡚Ұç਩Լ࿗çٌ။࿗ְè
ᄂྻ
■ ሸ‫֬ߋ׵‬༩๫ࡦҷƗႯ߃ࢿ૲࡬֍Ⴝ‫ށ‬ƗൗႯ١ѓƗႱߋ ֬MS/MSࡦҰƗનቇቒॕॠ֬‫׮‬ਏ‫ٺ‬༌ྺ౷
■ ඛओҗࠩ෕؎ঀƗ೫௽‫࠙૲ډ‬Ұਏ١૲֬ሠಙྦçᇞཊ ྦ‫ށ‬
■ ढ़॓ଷႯ֬ZSpray™սఞ࿩ঢ়ሷჾƗESIçAPCIçESCiçAPPIçASAP ְ۹ᇜঢ়ሷჾ଍൛ढ़࿑
\።፿ଗገ^
ҍ‫ٺ‬MRM๠֨"
Cone
No. Compound Chan Reaction
CE
Volt.
195.03 > 77.07
1
DMP
195.03 > 163.10
15
28
15
12
283.16 > 59.12
2
DMEP
28 3.16 > 207.11
18
14
18
8
311.16 > 45.0 9
ဟମ(ॊ) ഗႥ(ml/min)
%A
%B
ཎሣ
Βιβλιοθήκη Baidu
0.00
0.40
65
35
*
1.50
0.40
25
75
6
2.00
0.40
0
100
6
6.20
0.40
0
100
6
7.50
0.40
65
35
1
࣐ဩ฿࠙ƥ
10μL
\።፿ଗገ^
ᇿ໘ƥ ဩ௝໘؎ƥ ృ༨ಾ࠻ƥ ೗༨ಾ࠻ƥ ᄕྡྷ൏࡞ƥ
35˚C, 10˚C ACN H2O :ACN= 95:5 7.5‫ٺ‬ᇙ
3
DEEP
311.16 > 73.0 9
22
30
22
14
223.10 > 149.03
4
DEP
223.10 > 177.06
18
18
18
8
319.16 > 77.06
5
DPHP
319.16 > 225.11
20
30
20
12
......
18
DIDP
4 47.46 > 71.0 8
24
20
4 47.4 6 > 8 5.12
ႉਟࠕᇐ1ࡍњთ३ϩࢹ‫ݛ‬
ႉਟ ࠕᇐ1+18ᇜ ࠈ њ
ႉਟ ࠕᇐ1३ϩ
\።፿ଗገ^
ႉਟࠕᇐ2ࡍњთ३ϩࢹ‫ݛ‬
ႉਟ ࠕᇐ2+18ᇜ ࠈ њ
ႉਟࠕᇐ2३ϩ
ਈ᎖Waters ACQUITY UPLC H-Class HPLCࡼ‫ݷ‬ᔫऱजLjUPLCࡼᓳᏗቶถ ೉‫ݛ‬୤ᆥᄤ࣐ྡྷӏ݆‫ٺ‬༌Ɨࠎ١ٌा‫ن‬Ɨࠎ࣎࣎൥༦ߒවჴ г ༩ ๫ ‫ ئ‬ಾ ࠻ ֬ ਹ ࠊ ൗ Ⴏ Ɨ‫ ؾ‬Ⴢ फ़ ຳ ࠍ ֫ U P L C࠶ ඓ ւ দ ֬ ঀ ෕çۡਹ଀ ؎çۡ‫ٺ‬ঢ়؎֬ ྦ ୆Ɨ଱ી ໬ า ൞‫܋‬යAC QUIT Y UPLC H-Class༩๫൥୤଩ఴ຾၉֬࿑ᄻèACQUITY UPLC H-Class ༩ ๫ ൥ ၉ ั ࣣ ‫ݝ‬Ⴑߋ ֬ ༼ ࣐ ༩ ๫ Ɨक Ⴜ ව ჴ ಾ ࠻ ࠈ‫֬ ލ‬ਹ ࠊ ྦ ‫࡬ ދ‬ၥ ྦ ƗѰ ւ Ⴜ၉ ۸ ੇ ๠ ൛ ࣐ဩ ఝƗढ़ ൓ ཊU P LC‫ٺ‬ঢ় ֬༼࣐ྦ୆ḩ ḩۡ‫ٺ‬ঢ়؎çਹ଀ ؎‫ۡ ދ‬๠ਏƗ๤൏ߕГԂਛ ACQUITY༩๫෵Ы‫܋‬ಱ֬ଷႯྦ‫ދ‬ढ़॓ྦè ࿑ᄻACQUITY UPLC H-ClassƗ୤ढ़ၢᄤ૲ས໊দ֬LC௣ขഏࡆ࿊ ᄕ ྡྷ ཊႼ ֬ H P LC١ٌ ƗѰ ढ़ ൓ ཊ སU P LC‫ٺ‬ঢ় ֬ ໴ ‫ ڐ‬ሎ ߗè֙ ୤ ၉ ౔ ሠ Шः ࿉‫ ޱ‬Ɨ࠮ ढ़ൗ Ⴏ ࠩ ӵ ༩ ๫ ‫ ܄‬क ‫ ދ‬ढ़ ॓ ֬ ೫௽ ᇿ‫܄‬कЎ࣐ྡྷ١ٌሎߗ‫ދ‬١ٌा‫ن‬Ɨၢ࡬ߋ‫ੇ؏ݝ‬Ӹè ᄂྻ ‫ئ‬ಾ ࠻ ࠈ‫ ލ‬ƥQSMढ़ ࢃ ව ᇜ ಾ ࠻ φ ರ ‫ތ‬ቍ ‫ ࠎ ލ‬и৯ ࠈ‫ލ‬èൗ Ⴏ࿑஬֬ୄҍಾ࠻࿑ᄻًƗࢃढ़࿑ಾ࠻ছᅡ֥‫ئ‬չࣻᇜƗ١ ٌ‫ࡍ۾‬ਹࠊè ᆷ ࢫ ሆ തಃဩ ƥSM- F T N֬ ᆓ ੇ ್ ੥ ࣬ җႯሌ૑֬ ࠶ඓ Ɨᄤ ۡ ࿩৶༶୆‫ܛ‬Гᆪ࣡ಙ࣐֬ဩᆓ૨‫ྦچ‬Ɨढ़൓ཊۡ࣡؎ሆതƗ कႼࠥࡋ֬ဩ௝ߴ൳੸è ༶၉ք೫௽ᇿ໘མƥ໨૓֬ྔ൛UPLC೫௽ᇿࡍಪఝ‫ܼދ‬য়ఝ ၟ൓ཊਛњሠߋƗकႼၥ჆ҧቛç฿ཱི࠙֬ᇽ ‫׵‬൛ಾ࠻ხࡍಪఝƗൗ༩๫ᆴ࡞कႼཔ๤֬ཹ੸è೫௽ᇿხ
DEEP
14 .176 ਪ Э ‫ ࡑ ل‬ෝ‫ل‬Ɠ2-ѫ ࠕ ‫ۿ‬Ɣᴈ
DPHP
15.137 ਪ Э ‫ࡑل‬ෝ‫ ࠕ ק‬ᐅ ࠕ ᴈ
BBP
15. 311 ਪ Э ‫ ࡑ ل‬ෝ‫ ل‬ၺ‫ ק‬ᴈ
DIBP
15.464 ਪЭ ‫ࡑل‬ෝ‫ קل‬ᴈ
DBP
15.616 ਪ Э ‫ ࡑ ل‬ෝ‫ ل‬-Ɠ3 -‫ ק‬ဥ ࠕƔၠ ᴈ
■ ‫܄‬၃࠰਼༼֬‫ئ‬଍൛ࡦҰ୆৶၉՘ᄕྡྷ൏Ɨढ़๤൏࣐ྡྷ ‫ئ‬଍൛֬җࠩ
■ ሸ‫֬ߋ׵‬ၕఝႱߋთ‫׮‬ਏ١ٌा‫܄ن‬कƗ్࣡֬႒Ⴏ೏ ࡸ‫܄‬कЎƗ൨‫ލ‬Ⴏ߃֬า‫ٺ׮‬༌း౷è
■ ঀ෕֬ඛओҗࠩ୆৶ƗҗႯT-Wave™ாሖԄ࠶ඓç‫ئ‬଍൛ ঢ়ሷߋ࠶ඓçࠥྦঀ෕ሎߗ࠶ඓ
ყਛࢺਪЭ‫ࡑل‬ෝ࿾‫ٺ‬༌١ٌ֬‫ྗئ۾‬༖Ɨ
ಙГ൑௝็ࡍ࠻ࠎᆇ൑௝Юഭ൥‫ݪڕ‬ႼਪЭ‫ࡑل‬ෝ࿾৒༅ ᇐ֬၉۸๶࣬ः൥ൗႯ‫ٺ‬༌൴ؔ‫ؚ‬ఊ࣐ྡྷࡦҰè
໨૓ӏන֬ਪЭ‫ࡑل‬ෝ࿾൥၉৒ࢹ‫ܙ‬иࢧཔෂ֬ߋ‫ލ‬༅Ɨ ᄤ2011୔6ᄌƗᇖ‫ݚ‬໖ഺҍࢃ17ᇜਪЭ‫ࡑل‬ෝ࿾৒༅ᇐਠ್ û൑௝ᇖढ़୆ົٌ็ࡍ֬٫൑Ⴏ༅ᇐ‫ދ‬ၥশႯ֬൑௝็ࡍ ࠻ଇ֍ׂ੉ூüଇ֍Ɨ೉༶ƥ ਪЭ‫ࡑل‬ෝ‫ل‬2-ၠࠕ࠴ᴈDEHPç ਪЭ‫ࡑل‬ෝ‫ل‬ၺಫᴈDINPç ਪЭ‫ࡑل‬ෝ‫ل‬ЭᴈDPPç ਪЭ‫ࡑل‬ෝ‫ࡑل‬ᴈDMPç ਪЭ‫ࡑل‬ෝ‫ل‬ၠᴈDEPç ਪЭ‫ࡑل‬ෝ‫קل‬ᴈDBPç ਪЭ‫ࡑل‬ෝ‫ل‬༂ᴈDPPç ਪЭ‫ࡑل‬ෝ‫࠴ل‬ᴈDHXPç ਪЭ‫ࡑل‬ෝ‫ل‬ಫᴈDNPç ਪЭ‫ࡑل‬ෝ‫ل‬ၺ‫ק‬ᴈDIBPç ਪЭ‫ࡑل‬ෝ‫࠴ߓل‬ᴈDCHPç ਪЭ‫ࡑل‬ෝ‫ل‬ᆥྒྷᴈDNOPç ਪЭ‫ࡑل‬ෝ‫ࠕק‬ᐅࠕᴈBBPç ਪЭ‫ࡑل‬ෝ‫ل‬2-ࡑဥࠕၠᴈDMEPç ਪЭ‫ࡑل‬ෝ‫ل‬2-ၠဥࠕၠᴈDEEPç
ዹອᄋན)გᅭFDAऱज*ǖ ಃࠈᄒ‫ޱ‬ဩ௝1gƗ࣡ಙӲਏƗᇉ჆50mlಿਏ௥Ɨࡍ್ᄆ45ml ࡑՆƗӘഹѶᆘ֜30min৖ಖ‫ޱ‬ႯMeOH‫׮‬ಿ֥50mlèࣨᇉ ‫ޱ‬Ɨಃഏҍಾ၈ᄆ5mlᇉ჆ঢ়ྖܼᇖƗ჆3500rpmঢ়ྖ10min ಃഏ౩၈ሔ௥ևҰè‫ؚ‬჆ࠕᇐиࢧ‫ڶ‬ᄝ֬ဩ௝Ɨ‫ؚ‬჆฻ಃ ‫֬ޱ‬ဩ௝ढ़ၢҗႯ࣐၉ҋ֬‫ܬ‬པᑠಃࣱߋ൴ؔèӵࠗ෿çλ ᆨູ֬ཉè
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