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鑱�(li谩n)绯绘垜鍊�

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姘g浉鑹茶瓬璩�(zh矛)璀滆伅(li谩n)鐢ㄥ剙 GC-MS

鎮ㄧ暥(d膩ng)鍓嶆墍鍦ㄩ爜锛�棣栭爜 > 瑙f焙鏂规 > 姘g浉鑹茶瓬璩�(zh矛)璀滆伅(li谩n)鐢ㄥ剙 GC-MS

GC-MS 6800妾㈡脯閰掗涓殑鐢滆湝绱�

鐧�(f膩)甯冩棩鏈燂細2019/12/26 15:19:44  榛炴搳娆℃暩(sh霉)锛�34734

姒傝堪锛�鐢滆湝绱犳槸椋熷搧鐢熺敘(ch菐n)涓父鐢ㄧ殑鐢滃懗娣诲姞鍔戯紝鍏剁敎搴︽槸钄楃硸鐨�30锝�40鍊�,鎺у埗闄愰噺灏嶄汉鍊戠殑韬珨鍋ュ悍鏈夐噸瑕佹剰缇┿€傘€�GB 2760-2014 椋熷搧娣诲姞鍔戜娇鐢ㄦ(bi膩o)婧�(zh菙n)銆嬩腑鐢ㄤ簬鐣屽畾椋熷搧娣诲姞鍔戜娇鐢ㄨ寖鍦嶇殑椋熷搧鍒嗛绯荤当(t菕ng)锛岀櫧閰掑爆浜庤捀椁鹃厭锛屼笉鍏佽ū浣跨敤鐢滆湝绱犮€傛湰鏂规硶鍙冪収GB/T 5009.97-2003鍙婄浉闂�(gu膩n)鏂囩嵒璩囨枡锛屽皪鐧介厭涓殑鐢滆湝绱犵稉(j墨ng)鎻愬彇鍚庯紝鍦ㄥ啺娴存浠朵笅锛岃垏浜炵閰搁垑鐧�(f膩)鐢熼噸姘寲鍙嶆噳(y墨ng)鐢熸垚琛嶇敓鐗╃挵(hu谩n)宸遍唶浜炵閰搁叝锛岃鐢熺墿閫插叆姘g浉鑹茶瓬璩�(zh矛)璀滆伅(li谩n)鐢ㄥ剙閫茶鍒嗛洟妾㈡脯銆�


1 瀵﹂閮ㄥ垎

1.1  鍎€鍣ㄨ垏瑭﹀姂

姹熻槆澶╃憺鍎€鍣ㄨ偂浠芥湁闄愬叕鍙告埃鐩歌壊璀�-璩�(zh矛)璀滆伅(li谩n)鐢ㄥ剙锛�GC-MS 6800

鐢滆湝绱犳(bi膩o)婧�(zh菙n)鍎插倷婧舵恫锛氱ū鍙栦竴瀹氶噺鐨勭敎铚滅礌妯�(bi膩o)婧�(zh菙n)鍝侊紙绱斿害鐐�99.0锛咃級浜庡共鐕ュ閲忕摱涓紝鐢ㄦ按閰嶆垚1000m锝�/kg妯�(bi膩o)婧�(zh菙n)鍎插倷婧舵恫銆�

瑭﹀姂鍧囩偤鍎�(y艒u)绱氱磾锛岃│椹楃敤姘寸偤浜屾钂搁ぞ姘淬€�

1.2  鍎€鍣ㄥ伐浣滄浠�

1.2.1  姘g浉鑹茶瓬姊濅欢

DB-5姣涚窗绠¤壊璀滐紙30m 脳0.25mm,0.25um锛�锛涜級姘o細姘︽埃锛堢磾搴︾偤99.999锛咃級锛岃級姘f祦閲�1.0mL/min锛涢€叉ǎ鍙f韩搴�250鈩�锛岄€叉ǎ閲�1.0uL锛岄€叉ǎ鏂瑰紡鐐哄垎娴侀€叉ǎ,鍒嗘祦姣�10:1锛涚▼搴忓崌婧細鍒濆婧害鐐�40鈩�锛屼繚鎸佹檪闁�10min锛屼互25鈩�/min閫熺巼鍗囪嚦270鈩�锛屼繚鎸佹檪闁�5min銆�

1.2.2  璩�(zh矛)璀滄浠�

闆诲瓙杞熸搳闆㈠瓙婧愶紙EI锛�锛屽洓绱氭】婧害150鈩�锛屾帴鍙f韩搴�280鈩�锛涢噰闆嗘柟寮忕偤閬告搰闆㈠瓙鐩�(ji膩n)娓巸鎻忥紙SIM锛夛紝婧跺姂寤堕伈鏅傞枔6min,閬告搰3鍊嬬洠(ji膩n)娓洟瀛愯唱(zh矛)鑽锋瘮锛�m/z锛夌偤55,81,83銆�

1.3  瀵﹂鏂规硶锛堢暐锛�

绲�(ji茅)鏋滆垏瑷庤珫

2.1 鐗瑰緛鍜岄洟瀛愮殑閬告搰

鐢滆湝绱犵殑涓昏琛嶇敓鐗╃挵(hu谩n)宸遍唶浜炵閰搁叝浣滅偤瀹氭€у拰瀹氶噺锛屽鍦�1銆備繚鐣欐檪闁�8.511min.瀹氭€ч洟瀛愶紙m/z锛夌偤55,81,83銆傚畾閲忛洟瀛愮偤55銆傝唱(zh矛)璀滃湒瑕嬪湒2.


鍦�1銆佺敎铚滅礌琛嶇敓鐗╁湪绺介洟瀛愭祦鑹茶瓬鍦�

Figure 1銆� Cyclamate derivatives total ion chromatogram

 

鍦�2銆佺敎铚滅礌琛嶇敓鐗╃殑璩�(zh矛)璀滃湒

Figure 2銆� Cyclamate derivative spectrum

 鍦�3銆佺敎铚滅礌琛嶇敓鐗╁湪SIM鎺冩弿涓嬬殑闆㈠瓙娴佽壊璀滃湒

Figure 3銆� Cyclamate derivative SIM under scanning ion chromatogram

 

 鍦�4銆佺敎铚滅礌琛嶇敓鐗╁湪SIM鎺冩弿涓嬬殑璩�(zh矛)璀滃湒

Figure 4銆� Cyclamate derivative SIM under scanning spectrum

2.2 鍓嶈檿鐞嗘浠堕伕鎿�

2.2.1 琛嶇敓鏅傞枔閬告搰

婧�(zh菙n)纰哄惛鍙栫殑1ml鐢滆湝绱犲劜鍌欐恫婧舵恫鎸夌収涓婅堪琛嶇敓姝ラ閫茶琛嶇敓鍖�锛岀敎铚滅礌琛嶇敓鐗╂績搴︾偤200ug/mL锛岃鐢熷弽鎳�(y墨ng)鏅傞枔鍒嗗垾瑷�(sh猫)缃偤10min銆�20min銆�30min銆�40min銆�50min锛岃€冨療鍙嶆噳(y墨ng)鏅傞枔灏嶅弽鎳�(y墨ng)鐨勫奖闊�銆傜祼(ji茅)鏋滆〃鏄�锛岄毃钁楁檪闁撳緸10min鍗囪嚦30min锛岃鐢熺墿淇¤櫉闊挎噳(y墨ng)鍊奸€愭几澧炲姞锛岄毃钁楀弽鎳�(y墨ng)鏅傞枔鐨勫欢闀凤紝闊挎噳(y墨ng)鍊煎弽鑰屽嚭鐝�(xi脿n)闄嶄綆锛屽洜姝�锛岃鐢熷弽鎳�(y墨ng)婧害30min鏈€浣�銆�

2.2.2  纭吀婵冨害鐨勯伕鎿�

婧�(zh菙n)纰哄惛鍙栫殑1mL鐢滆湝绱犲劜鍌欐恫婧舵恫鎸夌収涓婅堪琛嶇敓姝ラ閫茶琛嶇敓鍖栵紝鐢滆湝绱犺鐢熺墿婵冨害鐐�200ug/mL锛屽啺娴村弽鎳�(y墨ng)姊濅欢涓�锛屽姞鍏�50g/L鐨勪簽纭濋吀閳夊拰鍒嗗垾鐐�50g/L锛�75g/L锛�100g/L锛�125g/L锛�150g/L銆傜祼(ji茅)鏋滆〃鏄�锛岄吀搴﹀緸50g/L鑷�100g/L锛屽弽鎳�(y墨ng)琛嶇敓鐗╀俊铏熼熆鎳�(y墨ng)鍊兼槑椤鍔�锛屾績搴﹀崌楂樻檪锛岄熆鎳�(y墨ng)鍊煎嚭鐝�(xi脿n)娓涘皯锛屽洜姝�锛屾渶绲傝鐢熷弽鎳�(y墨ng)閰稿害鐐�100g/L銆�

2.2.3 浜炵閰搁垑婵冨害灏嶈鐢熷弽鎳�(y墨ng)鐨勫奖闊�

婧�(zh菙n)纰哄惛鍙栫殑1ml鐢滆湝绱犲劜鍌欐恫婧舵恫鎸夌収涓婅堪琛嶇敓姝ラ閫茶琛嶇敓鍖栬鐢熷寲锛岀敎铚滅礌琛嶇敓鐗╂績搴︾偤200ug/mL锛屽啺娴村弽鎳�(y墨ng)姊濅欢涓�锛屽姞鍏�100g/L鐨勭~閰革紝鍜屽垎鍒ョ偤30g/L锛�50g/L锛�70g/L锛�90g/L浜炵閰搁垑銆傜祼(ji茅)鏋滆〃鏄�锛岄吀搴﹀緸30g/L鑷�50g/L锛屽弽鎳�(y墨ng)琛嶇敓鐗╀俊铏熼熆鎳�(y墨ng)鍊兼槑椤鍔�锛屾績搴﹀崌楂樻檪锛岄熆鎳�(y墨ng)鍊煎嚭鐝�(xi脿n)娓涘皯锛屽洜姝�锛屾渶绲備簽纭濋吀閳夎鐢熷弽鎳�(y墨ng)鐐�50g/L銆�

3 瀵﹂鏁�(sh霉)鎿�(j霉)

3.1  绮惧瘑搴﹀拰閲嶅京(f霉)鎬у椹�

婧�(zh菙n)纰虹Щ鍙栧劜鍌欐恫500uL浜庨洟蹇冪涓�锛岀敤姘村畾瀹�20mL鎸夌収涓婅堪妯�(bi膩o)妯h鐢熸椹熼€茶琛嶇敓鍖�锛岃鐢熺墿婵冨害鐐�100ug/mL锛屽钩琛屽埗鍌欏弽鎳�(y墨ng)娑�6娆★紝鐢�GC-MS娓畾?锛熺柧鐓呰媽顚嗘菛闂瑰櫓F(xi脿n)鎬т互鍙婄祫鍒嗕繚鐣欐檪闁撳拰宄伴潰绌嶇殑鐩稿皪妯�(bi膩o)婧�(zh菙n)鍋忓樊锛�6鍊嬪钩琛屾ǎ鐨勮瓬銆傜祼(ji茅)鏋滆〃鏄�锛屼繚鐣欐檪闁�RSD鐐�0.98%锛屽嘲闈㈢⿳RSD鐐�6.00%,锛屽叿楂斿椹楁暩(sh霉)鎿�(j霉)濡備笅琛�1鎵€绀� 銆�

琛�1銆侀噸寰�(f霉)鎬ф脯瑭︾祼(ji茅)鏋�

Table 1, repeatable test results

妯e搧鍚嶇ū

淇濈暀鏅傞枔

淇濈暀鏅傞枔RSD%

宄伴潰绌�

宄伴潰绌�RSD%

1

8.611

0.98%

96798

6.00%

2

8.518

99549

3

8.406

105518

4

8.431

99798

5

8.411

87708

6

8.410

96500


3.2  绶氭€ч棞(gu膩n)绯诲拰妾㈡脯闄�

婧�(zh菙n)纰哄惛鍙栨績搴︾偤10ug/mL鐨勭敎铚滅礌妯�(bi膩o)婧�(zh菙n)婧舵恫10ul浜�50ml闆㈠績绠′腑灏嶆噳(y墨ng)琛嶇敓鐗╂績搴﹀垎鍒ョ偤2ug/mL銆�10ug/mL銆�20ug/mL銆�100ug/mL銆�200ug/mL锛屾寜鐓т笂杩版(bi膩o)妯h鐢熷寲姝ラ閫茶琛嶇敓鍖�锛岄€茶绶氭€ф脯瑭�銆傚椹楁墍寰楃窔鎬ф柟绋嬬偤锛�y=940.43x-3525.57锛岀窔鎬х浉闂�(gu膩n)绯绘暩(sh霉)鐐�0.9984锛屽鍦�5鎵€绀�銆�

鍦�5. 绶氭€ч棞(gu膩n)绯诲湒

Figure 5锛�Linear

3.3 鍥炴敹鐜囨脯瑭�

閬告搰2mg/kg銆�50mg/kg銆�200mg/kg鐨勬(bi膩o)妯f坊鍔犳績搴�锛屽皪鏌愬搧鐗岀櫧閰掗€茶鍥炴敹鐜囧椹�锛屾瘡鍊嬫績搴﹀垎鍒ュ仛涓夋骞宠妯o紝鎸夎檿鐞嗘ǎ鍝佺殑鏂规硶铏曠悊鍔犳(bi膩o)鍚庣殑妯e搧骞舵脯瑭�锛岄噰鐢ㄥ妯�(bi膩o)娉曞畾閲忥紝娓│绲�(ji茅)鏋滃涓嬭〃2鎵€绀�銆�

婵冨害/mg/kg

鍥炴敹鐜�1/%

鍥炴敹鐜�2/%

鍥炴敹鐜�3/%

骞冲潎鍥炴敹鐜�/%

2

109.6

104.7

107.7

107.3

50

99.84

113.7

103.5

105.7

200

108.3

114.9

116.7

113.3

琛�2銆佸洖鏀剁巼娓│绲�(ji茅)鏋�

Table 2, the recovery test results

3.4 瀵﹂殯妯e搧娓│

鎸夌収涓婅堪妯e搧铏曠悊鏂规硶灏嶄笉鍚屽搧椤炵殑鐧介厭妯e搧閫茶鍓嶈檿鐞嗗拰琛嶇敓鍖栵紝浣跨敤GC-MS6800閫茶娓│锛屾脯瑭︾祼(ji茅)鏋滃涓嬭〃3鎵€绀猴細

妯e搧

鐢滆湝绱犲惈閲�/mg/kg

閰掓ǎ鍝�1

N.D.

閰掓ǎ鍝�2

N.D.

閰掓ǎ鍝�3

N.D.

閰掓ǎ鍝�4

N.D.

閰掓ǎ鍝�5

N.D.

娉細鈥淣.D鈥�琛ㄧず鈥�鏈鍑�鈥�

琛�3.銆侀厭涓敎铚滅礌鍚噺娓│绲�(ji茅)鏋�

 4 绲�(ji茅)璜�

鏈椹楅噰鐢�GCMS-6800锛屽湪SIM鎺冩弿妯″紡涓嬪皪閰掍腑鐨勭敎铚滅礌閫茶娓│鍜屽垎鏋�锛屾柟娉曠┅(w臎n)瀹氬彲闈�锛岀窔鎬ц寖鍦嶅ソ锛岄潏鏁忓害楂橈紝鍙楅洔璩�(zh矛)宄扮殑骞叉摼灏�锛岃兘澶犳湁鏁堝湴灏嶉厭涓殑鐢滆湝绱犻€茶瀹氭€у畾閲忓垎鏋�銆�


鐩搁棞(gu膩n)鐢�(ch菐n)鍝�

鑱�(li谩n)绯绘垜鍊�

浜嗚В鏇村瑭崇窗淇℃伅锛岃珛鑷撮浕
400-7102-888
闈炲伐浣滄檪闁撴湇鍕�(w霉)鐔辩窔
139 1323 1381
绲︽垜鍊戠暀瑷€
鍦ㄧ窔鐣欒█
寰俊鍞悗鏈嶅嫏(w霉)浜岀董纰�

400-7102-888