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�
2 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�