璁よ瘉锛欬span class="color3">宸ュ晢淇℃伅宸叉牳瀹濣/span>
鑱旂郴浜猴細 閿€鍞儴
鎽?nbsp; 瑕侊細寤虹珛浜嗕竴绉嶅湪绾胯秴涓寸晫钀冨彇銆佽秴涓寸晫鑹茶氨鍜岃川璋辫仈鐢ㄧ浉缁撳悎鐨勬娴嬪垎鏋愭柟娉曘€傛柟娉曞彇3mm鐨勫共鏂戠疆浜庢彁鍙栧櫒涓紝涓婃牱鍒嗘瀽銆傜粨鏋滄祴瀹?绉嶆瘨鐗╃殑绾挎€ц寖鍥村湪10锝?000ng/mL锛屽洖鏀剁巼鍧囧湪68.8锝?10.2涔嬮棿锛屾鍑洪檺鍦?锝?0ng/mL涔嬮棿銆傛暣涓柟娉曞叿鏈夌畝渚匡紝蹇€燂紝鍑嗙‘銆佺伒鏁忓害楂樼瓑鐗圭偣锛屼负妫€楠岃涓殑姣掔墿鎻愪緵浜嗕竴绉嶅叏鏂扮殑鍒嗘瀽鏂规硶銆侟br/>鍏抽敭璇嶏細瓒呬复鐣岃悆鍙栬秴涓寸晫鑹茶氨琛€姣掔墿
瓒呬复鐣岃悆鍙?SupercriticalFluidExtraction锛孲FE)鏄竴绉嶇墿鐞嗗垎绂诲拰绾寲鐨勬柟娉曪紝鍒╃敤鍘嬪姏鍜屾俯搴﹀CO2瓒呬复鐣屾祦浣撴憾瑙ｈ兘鍔涚殑褰卞搷鑰岃繘琛岀殑锛屽叾钀冨彇杩囩▼鐢辫悆鍙栧拰鍒嗙杩囩▼缁勫悎鑰屾垚銆傚湪瓒呬复鐣岀姸鎬佷笅锛屽皢CO2涓庡緟鍒嗙鐨勭墿璐ㄦ帴瑙︼紝浣垮叾鎸夌収娌哥偣楂樹綆銆佹瀬鎬уぇ灏忋€佸拰鍒嗗瓙閲忓ぇ灏忓皢鎴愬垎渚濇钀冨彇鍑烘潵銆傚搴斿悇鍘嬪姏鑼冨洿鎵€寰楀埌鐨勮悆鍙栫墿涓嶆槸缁濆鍗曚竴鐨勶紝浣嗗彲浠ラ€氳繃鎺у埗鏉′欢寰楀埌鏈€鐞嗘兂姣斾緥鐨勬贩鍚堟垚鍒嗭紝鐒跺悗鍊熷姪鍑忓帇銆佸崌娓╃殑鏂规硶浣胯秴涓寸晫娴佷綋鍙樻垚鏅€氭皵浣擄紝琚悆鍙栫墿璐ㄥ垯瀹屽叏鎴栧熀鏈瀽鍑猴紝浠庤€岃揪鍒板垎绂绘彁绾殑鐩殑銆傜洰鍓嶏紝瓒呬复鐣岃悆鍙栧拰瓒呬复鐣岃壊璋辨妧鏈湪澶╃劧鑽墿鎻愬彇銆佺幆澧冧繚鎶ょ瓑棰嗗煙鐨勫簲鐢ㄥ凡鏈夋姤閬擄紝浣嗗湪琛€娑蹭腑鐨勬瘨鐗╁垎鏋愭娴嬫姤閬撹緝灏戙€傛湰鐮旂┒閫氳繃瓒呬复鐣岃悆鍙栦华銆佽秴涓寸晫鑹茶氨鍜岃川璋辫仈鐢ㄧ浉缁撳悎锛岄€氳繃瀵硅秴涓寸晫钀冨彇鏉′欢杩涜浜嗘懜绱紝寤虹珛浜嗕竴绉嶅叏鏂扮殑鍦ㄧ嚎钀冨彇鍜屾恫璐ㄨ仈鐢ㄧ浉缁撳悎鐨勬瘨鐗╁垎鏋愭柟娉曘€傞€氳繃鏀瑰彉瓒呬复鐣岃悆鍙栫殑鏉′欢锛屾懜绱㈠嚭琛€娑蹭腑鍦拌タ娉€侀樋鏅攽浠戙€佷笁鍞戜粦銆佽壘鍙稿攽浠戙€佺鍩鸿タ娉拰姘瑗挎钞6绉嶅畨鐪犵被鑽墿鐨勬渶浣冲垎鏋愭柟娉曘€傝鏂规硶鍏锋湁鎿嶄綔绠€渚裤€佸揩閫熴€佹牱鍝佸鐞嗙畝鍗曘€佺伒鏁忓害楂樸€侀噸鐜版€уソ绛変紭鐐广€侟br/>1銆佹潗鏂欎笌鏂规硶
1.1銆佽瘯鍓傚拰鏉愭枡
鏍囧噯瀵圭収鍝侊細鍦拌タ娉?diazepam)銆侀樋鏅攽浠?alprazolam)銆佷笁鍞戜粦(triazolam)銆佽壘鍙稿攽浠?estazolam)銆佺鍩鸿タ娉?nitrazepam)銆佹隘纭濊タ娉?clonazepam)璐嚜鍏畨閮ㄧ墿璇侀壌瀹氫腑蹇冦€備互涓婄函鍝佸潎鐢ㄧ敳閱囬厤鍒舵垚1mg/mL 鐨勬爣鍑嗘憾娑层€俉hatman 903 DBS 鍗¤喘鑷猅閫氱敤鐢垫皵鍖荤枟闆嗗洟銆侟br/> Nexera UC 鍦ㄧ嚎瓒呬复鐣岃悆鍙?瓒呬复鐣岃壊璋变华(宀涙触)锛汱CMS-8040 涓夐噸鍥涙瀬鏉嗚川璋变华(宀涙触)銆侟br/>1.2銆佷华鍣ㄦ潯浠迭br/>1.2.1銆佽秴涓寸晫钀冨彇鏉′欢
1.2.2銆佽秴涓寸晫鑹茶氨-涓茶仈璐ㄨ氨浠潯浠迭br/>鑹茶氨鏌变负宀涙触GL鍏徃鑹茶氨鏌?Inetersil SIL 4.6 mm I.D.脳150 mmL.锛? 渭m)锛涙煴娓╋細40鈩冿紱娴佸姩鐩窤锛欳O2锛涙祦鍔ㄧ浉B(鏀规€у墏)锛氱敳閱囷紱娴侀€燂細3 mL/min锛涜悆鍙栧強娲楄劚绋嬪簭瑙佽〃1銆侟/span>
琛? 娴佸姩鐩稿拰姊害娲楄劚鏉′欢
| Time | Module | Commond | Value |
| 2.00 | SFE | Extraction Valve | Dynamic |
| 4.00 | SFE | End | |
| 4.00 | Pumps | Pump B Conc. | 10 |
| 4.01 | Pumps | Pump B Conc. | 20 |
| 10.00 | Pumps | Pump B Conc. | 20 |
| 18.00 | Pumps | Pump B Conc. | 100 |
| 20.01 | Pumps | Pump B Conc. | 100 |
| 20.01 | SFE | Wash | |
| 20.02 | Pumps | Shut Off Valve(Pump A) | Close |
| 21.99 | Pumps | Pump B Conc. | 100 |
| 22.00 | Pumps | Pump B Conc. | 0 |
| 22.00 | Pumps | Total Flow | 3 |
| 22.01 | Pumps | Total Flow | 0 |
| 22.02 | Pumps | Shut Off Valve(Pump A) | Open |
| 22.49 | Pumps | Shut Off Valve(Pump A) | Open(Pump On) |
| 22.50 | SFE | Extraction Valve | Static |
| 22.50 | Pumps | Total Flow | 0 |
| 22.51 | Pumps | Total Flow | 3 |
| 22.51 | SFE | Vent Valve | Vent |
| 25.50 | Controller | Stop |
璐ㄨ氨鏉′欢锛氱數鍠烽浘绂诲瓙婧愶紝姝ｇ瀛愭ā寮忥紱闆惧寲姘旀祦閫燂細3.0 L/min锛涘共鐕ュ櫒娴侀€燂細15 L/min锛汥L娓╁害锛?00鈩冿紱鍔犵儹妯″潡娓╁害锛?00鈩冿紱MRM 鍙傛暟瑙佽〃2銆侟/span>
琛? 鐩戞祴绂诲瓙瀵瑰拰纰版挒鑳键/span>
| 鍚嶇О | 淇濈暀鏃堕棿锛坢in锛堻/span> | 瀹氶噺绂诲瓙瀵更/span> | 瀹氭€х瀛愬 | 纰版挒鑳介噺锛坋V锛堻br/> 瀹氶噺/瀹氭€?/span> |
| 鍦拌タ娉?/span> | 5.550 | 285.10 > 193.10 | 285.10 > 154.10 | -32/-28 |
| 纭濊タ娉?/span> | 6.353 | 282.05 > 236.10 | 282.05 > 207.25 | -24/-35 |
| 姘瑗挎钞 | 6.474 | 316.00 > 270.05 | 316.00 > 241.05 | -25/-37 |
| 鑹惧徃鍞戜粦 | 9.408 | 295.10 > 267.05 | 295.10 > 267.05 | -25/-45 |
| 闃挎櫘鍞戜粦 | 10.231 | 309.10 > 205.10 | 309.10 > 281.00 | -45/-25 |
| 涓夊攽浠慄/span> | 10.902 | 343.00 > 308.05 | 343.00 > 238.90 | -28/-35 |
1.3銆佹牱鍝佸鐞咟br/>鏍囧噯鍝佺殑鍒跺锛氬皢1000 ng/mL 鐨勬爣鍑嗘贩鍚堟恫锛屼娇鐢ㄧ敳閱囩█閲婅嚦500銆?00銆?00銆?0銆?0 ng/mL鐨勬爣鍑嗘憾娑诧紝鐢ㄤ簬鏍″噯鏇茬嚎鐨勫埗浣溿€傛瘡浠芥爣鍑嗘憾娑插彇20渭L 鐐规牱鍒癢hatman 903 DBS 鍗′笂銆傚娓╂櫨骞插悗鎵撳瓟鍙栫洿寰? mm 鐨勫共鏂戠疆浜庢彁鍙栧櫒涓紝涓婃牱鍒嗘瀽銆侟br/> 鏍峰搧鐨勫埗澶囷細鍙?0 渭L 浜鸿鐐规牱鍒癢hatman 903 DBS 鍗′笂锛屽娓╂櫨骞插悗鎵撳瓟鍙栫洿寰? mm 鐨勫共鏂戠疆浜庢彁鍙栧櫒涓紝涓婃牱鍒嗘瀽銆侟br/>2銆佺粨鏋滀笌璁ㄨ
2.1銆佽秴涓寸晫钀冨彇鏉′欢鐨勪紭鍖朁br/>璇曢獙浠ヨ悆鍙栨敼鎬у墏鐨勭敤閲忋€佽悆鍙栧帇鍔涘拰钀冨彇娓╁害涓哄彉閲忥紝浠ョ洰鏍囩墿鐨勫嘲闈㈢Н涓鸿瘎浠疯悆鍙栨晥鐜囩殑浼樺姡銆侟br/>2.1.1銆佽悆鍙栨敼鎬у墏鐨勯€夋嫨
鐢变簬鐩爣鐗╄川鏋佹€ц緝澶э紝浠呬娇鐢ㄥ急鏋佹€х殑CO2寰堥毦灏嗙洰鏍囩墿璐ㄦ彁鍙栧嚭鏉ワ紝鍥犳锛屽姞鍏ラ€傞噺鐨勬敼鎬у墏鏄瑕侀€夋嫨銆傛湰璇曢獙浣跨敤鐢查唶浣滀负鏀规€у墏锛岃€冨療浜嗙敳閱囩殑鐢ㄩ噺涓?%銆?0%鍜?5%瀵规彁鍙栭噺鐨勫奖鍝嶃€傜粨鏋滄樉绀?0%鐨勭敤閲忔渶浣炽€傜敳閱囩敤閲忎笌鐩爣姣掔墿宄伴潰绉叧绯诲鍥炬墍绀恒€侟/span>
2.1.2銆佽悆鍙栧帇鍔涚殑閫夋嫨
鑲栬绉€绛夊湪鐮旂┒瓒呬复鐣岃悆鍙栫敓鐗╃⒈鏃跺彂鐜帮紝閫傚綋鎻愰珮钀冨彇鍘嬪姏鑳芥樉钁楁彁楂樿秴涓寸晫娴佷綋鐨勬憾瑙ｈ兘鍔涖€傛湰璇曢獙涓€冨療浜?0 MPa銆?0 Mp 鍜?0 MPa 钀冨彇鍘嬪姏涓嬶紝6 绉嶆瘨鐗╃殑宄伴潰绉€傜粨鏋滃彂鐜帮紝褰撹悆鍙栧帇鍔涗粠10 MPa 澧炲姞鍒?5 MPa 鏃讹紝鎻愬彇鏁堢巼鏈夋槑鏄剧殑鎻愰珮锛屾墍鏈夋瘨鐗╃殑宄伴潰绉槑鏄炬彁楂橈紝鏈変簺鐢氳嚦鎻愰珮浜?-3 鍊嶃€傚綋缁х画鎻愰珮鎻愬彇鍘嬪姏鍒?0 MPa 鏃讹紝鑹惧徃鍞戜粦銆侀樋鏅攽浠戝拰涓夊攽浠戠殑宄伴潰绉户缁鍔狅紱鑰屽叾浠栨瘨鐗╃殑鍛堢幇涓嬮檷瓒嬪娍锛屼笉杩囦笅闄嶇殑涓嶆槸闈炲父鐨勬槑鏄俱€侟/span>
2.1.3銆佽悆鍙栨俯搴︾殑閫夋嫨
鍦ㄥ叾浠栨潯浠朵笉鍙樻儏鍐典笅锛岃€冨療浜嗚悆鍙栨俯搴﹀琛€涓瘨鐗╃殑钀冨彇鑳藉姏銆備粠鍥捐悆鍙栨俯搴﹀宄伴潰绉殑鏇茬嚎鍙互鐪嬪嚭锛屽瓨鍦ㄦ渶浣崇殑钀冨彇娓╁害銆備笖锛屼粠鍥句腑鏄庢樉鐪嬪嚭锛屽浜庡鏁版瘨鐗╋紝褰撹悆鍙栨俯搴﹁揪鍒?0鈩冩椂锛屽嘲闈㈢Н鏈€灏忋€侟/span>
2.2銆丮RM 鑹茶氨鍥近br/>200 ng/mL 浜鸿鍔犳爣鏍峰搧鐨勮壊璋卞浘濡備笅鍥炬墍绀猴紝6绉嶆瘨鐗╁緱鍒颁簡杈冨ソ鐨勫垎绂汇€備娇鐢ㄥ湪绾縎FE-SFC绯荤粺锛屼粠鎻愬彇鍒板垎绂诲垎鏋愪粎闇€瑕?5鍒嗛挓銆傚ぇ澶ц妭鐪佷簡鏁翠釜鍒嗘瀽鍛ㄦ湡銆侟/span>
2.3銆佹鍑洪檺銆佺嚎鎬ц寖鍥村拰鍥炴敹鐜嘃br/>鐢ㄦ墍寤虹珛鐨勬柟娉曡繘琛屼簡涓€浜涘垎鏋愮墿瀹氶噺鍒嗘瀽鐨勭嚎鎬у叧绯诲拰鍥炴敹鐜囩殑鑰冨療銆傚垎鍒湪 DBS 鍗′笂鍔犲叆涓嶅悓娴撳害鐨勬爣鍑嗘憾娑茶繘琛屽垎鏋愶紝灏嗗垎鏋愮墿鑹茶氨宄伴潰绉瘮涓庢祿搴﹁繘琛屽洖褰掞紝寰楃嚎鎬ф柟绋嬪強鐩稿叧绯绘暟瑙佽〃3銆傛祴璇?00 ng/mL 娴撳害鐨勪汉琛€鍔犳爣鏍峰搧锛屽钩琛屾祴瀹?娆★紝鍙栧钩鍧囧€间綔涓哄洖鏀剁巼缁撴灉锛屽悓鏃惰绠?娆℃牱鍝佺殑鐩稿鏍囧噯鍋忓樊浣滀负绮惧瘑搴﹁瘎浠凤紝浠ヤ笂瀹為獙缁撴灉涓€骞跺垪鍏ヨ〃3涓€傛牴鎹垎鏋愮墿宄伴珮涓庡惈閲忔垚姝ｆ瘮锛岃绠楀嚭鍒嗘瀽鐗╄壊璋卞嘲楂樼浉褰撲簬鍩虹嚎鍣煶寮哄害涓夊€嶆鏉愪腑鍒嗘瀽鐗╂祿搴︺€傚悇鑽墿鐨勬鍑洪檺(S/N=3)鍦?锝?0 ng/mL 涔嬮棿銆侟/span>
琛? 6 绉嶅父瑙侀晣闈欒嵂鐗╃殑绾挎€у叧绯诲拰鍥炴敹鐜嘃/span>
| 鑽墿缁勫垎 | tR(min) | 绾挎€ц寖鍥滁br/> (ng/mL) | 鐩稿叧绯绘暟 (R2) |
LOD (ng/mL) |
鍥炴敹鐜嘃br/> (%) | RSD (%锛宯=3) |
| 鍦拌タ娉?/span> | 5.338 | 10锝?00 | 0.994 | 2 | 99.1 | 13.6 |
| 纭濊タ娉?/span> | 6.458 | 50锝?000 | 0.992 | 8 | 110.2 | 15.4 |
| 姘瑗挎钞 | 6.574 | 50锝?000 | 0.996 | 8 | 94.4 | 20.2 |
| 鑹惧徃鍞戜粦 | 9.962 | 10锝?00 | 0.999 | 1 | 78 | 16.7 |
| 闃挎櫘鍞戜粦 | 10.828 | 10锝?00 | 0.996 | 1 | 107.9 | 18.8 |
| 涓夊攽浠慄/span> | 11.733 | 50锝?000 | 0.992 | 10 | 68.8 | 18.4 |
3銆佸皬缁掽br/> 鏈枃寤虹珛浜嗕娇鐢ㄨ秴涓寸晫钀冨彇-瓒呬复鐣岃壊璋辫川璋卞湪绾挎彁鍙栧拰鍒嗘瀽浜鸿涓殑6绉嶅畨鐪犵被鐨勬柟娉曘€傝鏂规硶鍏锋湁鑷姩鍖栫▼搴﹂珮銆佹彁鍙栨椂闂寸煭銆佹牱鍝佺敤閲忓皯銆佺幆澧冩薄鏌撳皬绛変紭鐐癸紝鎿嶄綔鐪佹椂鐪佸姏锛岃€屼笖璇ユ柟娉曞鍒嗘瀽浜哄憳鐨勮姹傝緝浣庛€佺簿瀵嗗害銆佹鍑洪檺绛夊悇椤规柟娉曞鎸囨爣鍧囩鍚堟硶搴瀛︽瘨鐗╁垎鏋愮殑瑕佹眰锛屼负妫€楠岃涓殑姣掔墿鍒嗘瀽妫€娴嬫彁渚涗簡涓€绉嶅叏鏂扮殑蹇€熸彁鍙栧垎鏋愭柟娉曘€侟/span>