¸ÅÊö£ºÌðÃÛËØÊÇʳƷÉú²úÖг£ÓõÄÌðζÌí¼Ó¼Á£¬ÆäÌð¶ÈÊÇÕáÌǵÄ30¡«40±¶,¿ØÖÆÏÞÁ¿¶ÔÈËÃǵÄÉíÌ彡¿µÓÐÖØÒªÒâÒå¡£¡¶GB 2760-2014 ʳƷÌí¼Ó¼ÁʹÓñê×¼¡·ÖÐÓÃÓڽ綨ʳƷÌí¼Ó¼ÁʹÓùæÄ£µÄʳƷ·ÖÀàϵͳ£¬°×¾ÆÊôÓÚÕôÁ󾯣¬²»ÔÊÐíʹÓÃÌðÃÛËØ¡£±¾ÒªÁì²ÎÕÕGB/T 5009.97-2003¼°Ïà¹ØÎÄÏ××ÊÁÏ£¬¶Ô°×¾ÆÖеÄÌðÃÛËØ¾ÌáÈ¡ºó£¬ÔÚ±ùÔ¡Ìõ¼þÏ£¬ÓëÑÇÏõËáÄÆ±¬·¢Öصª»¯·´Ó¦Éú³ÉÑÜÉúÎï»·¼º´¼ÑÇÏõËáõ¥£¬ÑÜÉúÎï½øÈëÆøÏàÉ«Æ×ÖÊÆ×ÁªÓÃÒǽøÐÐÊèÉ¢¼ì²â¡£
1 ʵÑ鲿·Ö
1.1 ÒÇÆ÷ÓëÊÔ¼Á
ÃÀʨ¹ó±ö»áÆøÏàÉ«Æ×-ÖÊÆ×ÁªÓÃÒÇ£ºGC-MS 6800
ÌðÃÛËØ±ê×¼´¢±¸ÈÜÒº£º³ÆÈ¡Ò»¶¨Á¿µÄÌðÃÛËØ±ê׼Ʒ£¨´¿¶ÈΪ99.0£¥£©ÓÚ¸ÉÔïÈÝÁ¿Æ¿ÖУ¬ÓÃË®Åä³É1000m£ç/kg±ê×¼´¢±¸ÈÜÒº¡£
ÊÔ¼Á¾ùΪÓż¶´¿£¬ÊÔÑéÓÃˮΪ¶þ´ÎÕôÁóË®¡£
1.2 ÒÇÆ÷ÊÂÇéÌõ¼þ
1.2.1
ÆøÏàÉ«Æ×Ìõ¼þ
DB-5ëϸ¹ÜÉ«Æ×£¨30m ¡Á0.25mm,0.25um£©£»ÔØÆø£ºº¤Æø£¨´¿¶ÈΪ99.999£¥£©£¬ÔØÆøÁ÷Á¿1.0mL/min£»½øÑù¿ÚζÈ250¡æ£¬½øÑùÁ¿1.0uL£¬½øÑù·½·¨Îª·ÖÁ÷½øÑù,·ÖÁ÷±È10:1£»³ÌÐòÉýΣº³õʼζÈΪ40¡æ£¬¼á³Öʱ¼ä10min£¬ÒÔ25¡æ/minËÙÂÊÉýÖÁ270¡æ£¬¼á³Öʱ¼ä5min¡£
1.2.2
ÖÊÆ×Ìõ¼þ
µç×Óºä»÷Àë×ÓÔ´£¨EI£©£¬ËﶏËζÈ150¡æ£¬½Ó¿ÚζÈ280¡æ£»ÊÕÂÞ·½·¨ÎªÑ¡ÔñÀë×Ó¼à²âɨÃ裨SIM£©£¬ÈܼÁÑÓ³Ùʱ¼ä6min,Ñ¡Ôñ3¸ö¼à²âÀë×ÓÖʺɱȣ¨m/z£©Îª55,81,83¡£
1.3 ʵÑéÒªÁ죨ÂÔ£©
2 ½á¹ûÓëÌÖÂÛ
2.1 ÌØÕ÷ºÍÀë×ÓµÄÑ¡Ôñ
ÌðÃÛËØµÄÖ÷ÒªÑÜÉúÎï»·¼º´¼ÑÇÏõËáõ¥×÷Ϊ¶¨ÐԺͶ¨Á¿£¬Èçͼ1¡£±£´æÊ±¼ä8.511min.¶¨ÐÔÀë×Ó£¨m/z£©Îª55,81,83¡£¶¨Á¿Àë×ÓΪ55¡£ÖÊÆ×ͼ¼ûͼ2.

ͼ1¡¢ÌðÃÛËØÑÜÉúÎïÔÚ×ÜÀë×ÓÁ÷É«Æ×ͼ
Figure 1¡¢ Cyclamate derivatives total ion
chromatogram
ͼ2¡¢ÌðÃÛËØÑÜÉúÎïµÄÖÊÆ×ͼ
Figure 2¡¢ Cyclamate derivative spectrum
ͼ3¡¢ÌðÃÛËØÑÜÉúÎïÔÚSIMɨÃèϵÄÀë×ÓÁ÷É«Æ×ͼ
Figure 3¡¢ Cyclamate
derivative SIM under scanning ion chromatogram
ͼ4¡¢ÌðÃÛËØÑÜÉúÎïÔÚSIMɨÃèϵÄÖÊÆ×ͼ
Figure 4¡¢ Cyclamate derivative SIM
under scanning spectrum
2.2 ǰ´¦ÀíÌõ¼þÑ¡Ôñ
2.2.1 ÑÜÉúʱ¼äÑ¡Ôñ
׼ȷÎüÈ¡µÄ1mlÌðÃÛËØ´¢±¸ÒºÈÜҺƾ¾ÝÉÏÊöÑÜÉú°ì·¨½øÐÐÑÜÉú»¯£¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL£¬ÑÜÉú·´Ó¦Ê±¼ä»®·ÖÉèÖÃΪ10min¡¢20min¡¢30min¡¢40min¡¢50min£¬¿¼²ì·´Ó¦Ê±¼ä¶Ô·´Ó¦µÄÓ°Ïì¡£½á¹û±êÃ÷£¬Ëæ×Åʱ¼ä´Ó10minÉýÖÁ30min£¬ÑÜÉúÎïÐźÅÏìÓ¦ÖµÖð½¥Ôö¼Ó£¬Ëæ×Å·´Ó¦Ê±¼äµÄÑÓ³¤£¬ÏìÓ¦Öµ·´¶ø·ºÆð½µµÍ£¬Òò´Ë£¬ÑÜÉú·´Ó¦Î¶È30min×î¼Ñ¡£
2.2.2
ÁòËáŨ¶ÈµÄÑ¡Ôñ
׼ȷÎüÈ¡µÄ1mLÌðÃÛËØ´¢±¸ÒºÈÜҺƾ¾ÝÉÏÊöÑÜÉú°ì·¨½øÐÐÑÜÉú»¯£¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL£¬±ùÔ¡·´Ó¦Ìõ¼þÏ£¬¼ÓÈë50g/LµÄÑÇÏõËáÄÆºÍ»®·ÖΪ50g/L£¬75g/L£¬100g/L£¬125g/L£¬150g/L¡£½á¹û±êÃ÷£¬Ëá¶È´Ó50g/LÖÁ100g/L£¬·´Ó¦ÑÜÉúÎïÐźÅÏìÓ¦ÖµÃ÷ÏÔÔö¼Ó£¬Å¨¶ÈÉý¸ßʱ£¬ÏìÓ¦Öµ·ºÆð¼õÉÙ£¬Òò´Ë£¬×îÖÕÑÜÉú·´Ó¦Ëá¶ÈΪ100g/L¡£
2.2.3 ÑÇÏõËáįō¶È¶ÔÑÜÉú·´Ó¦µÄÓ°Ïì
׼ȷÎüÈ¡µÄ1mlÌðÃÛËØ´¢±¸ÒºÈÜҺƾ¾ÝÉÏÊöÑÜÉú°ì·¨½øÐÐÑÜÉú»¯ÑÜÉú»¯£¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL£¬±ùÔ¡·´Ó¦Ìõ¼þÏ£¬¼ÓÈë100g/LµÄÁòËᣬºÍ»®·ÖΪ30g/L£¬50g/L£¬70g/L£¬90g/LÑÇÏõËáÄÆ¡£½á¹û±êÃ÷£¬Ëá¶È´Ó30g/LÖÁ50g/L£¬·´Ó¦ÑÜÉúÎïÐźÅÏìÓ¦ÖµÃ÷ÏÔÔö¼Ó£¬Å¨¶ÈÉý¸ßʱ£¬ÏìÓ¦Öµ·ºÆð¼õÉÙ£¬Òò´Ë£¬×îÖÕÑÇÏõËáÄÆÑÜÉú·´Ó¦Îª50g/L¡£
3 ʵÑéÊý¾Ý
3.1 ¾«ÃܶȺÍÖØ¸´ÐÔʵÑé
×¼È·ÒÆÈ¡´¢±¸Òº500uLÓÚÀëÐĹÜÖУ¬ÓÃË®¶¨ÈÝ20mLƾ¾ÝÉÏÊö±êÑùÑÜÉú°ì·¨½øÐÐÑÜÉú»¯£¬ÑÜÉúÎïŨ¶ÈΪ100ug/mL£¬Æ½ÐÐÖÆ±¸·´Ó¦Òº6´Î£¬ÓÃGC-MS²â¶¨¡£¿¼²ìÑÜÉúÒªÁìµÄÖØÏÖÐÔÒÔ¼°×é·Ö±£´æÊ±¼äºÍ·åÃæ»ýµÄÏà¶Ô±ê׼ƫ²î£¬6¸öƽÐÐÑùµÄÆ×¡£½á¹û±êÃ÷£¬±£´æÊ±¼äRSDΪ0.98%£¬·åÃæ»ýRSDΪ6.00%,£¬¾ßÌåʵÑéÊý¾ÝÈçϱí1Ëùʾ ¡£
±í1¡¢Öظ´ÐÔ²âÊÔ½á¹û
Table 1, repeatable test results
|
ÑùÆ·Ãû³Æ
|
±£´æÊ±¼ä
|
±£´æÊ±¼äRSD%
|
·åÃæ»ý
|
·åÃæ»ýRSD%
|
|
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 ÏßÐÔ¹ØÏµºÍ¼ì²âÏÞ
׼ȷÎüȡŨ¶ÈΪ10ug/mLµÄÌðÃÛËØ±ê×¼ÈÜÒº10ulÓÚ50mlÀëÐĹÜÖжÔÓ¦ÑÜÉúÎïŨ¶È»®·ÖΪ2ug/mL¡¢10ug/mL¡¢20ug/mL¡¢100ug/mL¡¢200ug/mL£¬Æ¾¾ÝÉÏÊö±êÑùÑÜÉú»¯°ì·¨½øÐÐÑÜÉú»¯£¬½øÐÐÏßÐÔ²âÊÔ¡£ÊµÑéËùµÃÏßÐÔ·½³ÌΪ£ºy=940.43x-3525.57£¬ÏßÐÔÏà¹ØÏµÊýΪ0.9984£¬Èçͼ5Ëùʾ¡£
ͼ5. ÏßÐÔ¹ØÏµÍ¼
Figure 5£¬Linear
3.3 ½ÓÄÉÂʲâÊÔ
Ñ¡Ôñ2mg/kg¡¢50mg/kg¡¢200mg/kgµÄ±êÑùÌí¼ÓŨ¶È£¬¶ÔÄ³Æ·ÅÆ°×¾Æ½øÐнÓÄÉÂÊʵÑ飬ÿ¸öŨ¶È»®·Ö×öÈý´ÎƽÐÐÑù£¬°´´¦ÀíÑùÆ·µÄÒªÁì´¦Àí¼Ó±êºóµÄÑùÆ·²¢²âÊÔ£¬½ÓÄÉÍâ±ê·¨¶¨Á¿£¬²âÊÔ½á¹ûÈçϱí2Ëùʾ¡£
|
Ũ¶È/mg/kg
|
½ÓÄÉÂÊ1/%
|
½ÓÄÉÂÊ2/%
|
½ÓÄÉÂÊ3/%
|
ƽ¾ù½ÓÄÉÂÊ/%
|
|
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
|
±í2¡¢½ÓÄÉÂʲâÊÔ½á¹û
Table 2, the recovery test results
3.4 ʵ¼ÊÑùÆ·²âÊÔ
ƾ¾ÝÉÏÊöÑùÆ·´¦ÀíÒªÁì¶Ô²î±ðÆ·ÀàµÄ°×¾ÆÑùÆ·½øÐÐǰ´¦ÀíºÍÑÜÉú»¯£¬Ê¹ÓÃGC-MS6800½øÐвâÊÔ£¬²âÊÔ½á¹ûÈçϱí3Ëùʾ£º
|
ÑùÆ·
|
ÌðÃÛËØº¬Á¿/mg/kg
|
|
¾ÆÑùÆ·1
|
N.D.
|
|
¾ÆÑùÆ·2
|
N.D.
|
|
¾ÆÑùÆ·3
|
N.D.
|
|
¾ÆÑùÆ·4
|
N.D.
|
|
¾ÆÑùÆ·5
|
N.D.
|
×¢£º¡°N.D¡±ÌåÏÖ¡°Î´¼ì³ö¡±
±í3.¡¢¾ÆÖÐÌðÃÛËØº¬Á¿²âÊÔ½á¹û
4 ½áÂÛ
±¾ÊµÑé½ÓÄÉGCMS-6800£¬ÔÚSIMɨÃèģʽ϶ԾÆÖеÄÌðÃÛËØ½øÐвâÊÔºÍÆÊÎö£¬ÒªÁìÎȶ¨¿É¿¿£¬ÏßÐÔ¹æÄ£ºÃ£¬ÁéÃô¶È¸ß£¬ÊÜÔÓÖÊ·åµÄ×ÌÈÅС£¬Äܹ»ÓÐЧµØ¶Ô¾ÆÖеÄÌðÃÛËØ½øÐж¨ÐÔ¶¨Á¿ÆÊÎö¡£