ΰµÂ¹ú¼Ê1946¹Ù·½Íø

ÊÖ³Öʽ¹âÆ×ÒÇÊÖ³ÖʽºÏ½ðÆÊÎöÒǺϽðÆÊÎöÒÇ
¹ÉƱ´úÂ룺300165 ÆóÒµÓÊÏä Ͷ×ÊÕß¹ØÏµ
ΤµÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

ʳÎïÇå¾²

ÄúÄ¿½ñËùÔÚÒ³£ºÊ×Ò³ > ½â¾ö¼Æ»® > ʳÎïÇå¾²

GC-MS 6800¼ì²â¾ÆÀàÖеÄÌðÃÛËØ

Ðû²¼ÈÕÆÚ£º2019/12/26 15:19:44  µã»÷´ÎÊý£º46904

¸ÅÊö£ºÌðÃÛËØÊÇʳÎïÉú²úÖг£ÓõÄÌðζÌí¼Ó¼Á £¬ÆäÌð¶ÈÊÇÕáÌǵÄ30¡«40±¶,¿ØÖÆÏÞÁ¿¶ÔÈËÃǵÄÉíÌ念½¡ÓÐÖ÷ÒªÒâÒå ¡£¡¶GB 2760-2014 ʳÎïÌí¼Ó¼ÁʹÓñê×¼¡·ÖÐÓÃÓڽ綨ʳÎïÌí¼Ó¼ÁʹÓùæÄ£µÄʳÎï·ÖÀàϵͳ £¬°×¾ÆÊôÓÚÕôÁó¾Æ £¬²»ÔÊÐíʹÓÃÌðÃÛËØ ¡£±¾ÒªÁì²ÎÕÕGB/T 5009.97-2003¼°Ïà¹ØÎÄÏ××ÊÁÏ £¬¶Ô°×¾ÆÖеÄÌðÃÛËØ¾­ÌáÈ¡ºó £¬ÔÚ±ùÔ¡Ìõ¼þÏ £¬ÓëÑÇÏõËáÄÆ±¬·¢Öصª»¯·´Ó¦ÌìÉúÑÜÉúÎï»·¼º´¼ÑÇÏõËáõ¥ £¬ÑÜÉúÎï½øÈëÆøÏàÉ«Æ×ÖÊÆ×ÁªÓÃÒǾÙÐÐÊèÉ¢¼ì²â ¡£


1 ʵÑ鲿·Ö

1.1  ÒÇÆ÷ÓëÊÔ¼Á

ΰµÂ¹ú¼Ê1946¹Ù·½ÍøÆøÏàÉ«Æ×-ÖÊÆ×ÁªÓÃÒÇ£ºGC-MS 6800

ÌðÃÛËØ±ê×¼´¢±¸ÈÜÒº£º³ÆÈ¡Ò»¶¨Á¿µÄÌðÃÛËØ±ê׼Ʒ£¨´¿¶ÈΪ99.0£¥£©ÓÚ¸ÉÔïÈÝÁ¿Æ¿ÖÐ £¬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£©

Ч¹ûÓëÌÖÂÛ

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.

ΤµÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

ͼ1¡¢ÌðÃÛËØÑÜÉúÎïÔÚ×ÜÀë×ÓÁ÷É«Æ×ͼ

Figure 1¡¢ Cyclamate derivatives total ion chromatogram

 Î¤µÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

ͼ2¡¢ÌðÃÛËØÑÜÉúÎïµÄÖÊÆ×ͼ

Figure 2¡¢ Cyclamate derivative spectrum

ΤµÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

 Í¼3¡¢ÌðÃÛËØÑÜÉúÎïÔÚSIMɨÃèϵÄÀë×ÓÁ÷É«Æ×ͼ

Figure 3¡¢ Cyclamate derivative SIM under scanning ion chromatogram

 Î¤µÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

 Í¼4¡¢ÌðÃÛËØÑÜÉúÎïÔÚSIMɨÃèϵÄÖÊÆ×ͼ

Figure 4¡¢ Cyclamate derivative SIM under scanning spectrum

2.2 ǰ´¦Öóͷ£Ìõ¼þÑ¡Ôñ

2.2.1 ÑÜÉúʱ¼äÑ¡Ôñ

׼ȷÎüÊÕµÄ1mlÌðÃÛËØ´¢±¸ÒºÈÜҺƾ֤ÉÏÊöÑÜÉú°ì·¨¾ÙÐÐÑÜÉú»¯ £¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL £¬ÑÜÉú·´Ó¦Ê±¼ä»®·ÖÉèÖÃΪ10min¡¢20min¡¢30min¡¢40min¡¢50min £¬¿¼²ì·´Ó¦Ê±¼ä¶Ô·´Ó¦µÄÓ°Ïì ¡£Ð§¹ûÅú×¢ £¬Ëæ×Åʱ¼ä´Ó10minÉýÖÁ30min £¬ÑÜÉúÎïÐźÅÏìÓ¦ÖµÖð½¥ÔöÌí £¬Ëæ×Å·´Ó¦Ê±¼äµÄÑÓÉì £¬ÏìÓ¦Öµ·´¶ø·ºÆð½µµÍ £¬Òò´Ë £¬ÑÜÉú·´Ó¦Î¶È30min×î¼Ñ ¡£

2.2.2  ÁòËáŨ¶ÈµÄÑ¡Ôñ

׼ȷÎüÊÕµÄ1mLÌðÃÛËØ´¢±¸ÒºÈÜҺƾ֤ÉÏÊöÑÜÉú°ì·¨¾ÙÐÐÑÜÉú»¯ £¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL £¬±ùÔ¡·´Ó¦Ìõ¼þÏ £¬¼ÓÈë50g/LµÄÑÇÏõËáÄÆºÍ»®·ÖΪ50g/L £¬75g/L £¬100g/L £¬125g/L £¬150g/L ¡£Ð§¹ûÅú×¢ £¬Ëá¶È´Ó50g/LÖÁ100g/L £¬·´Ó¦ÑÜÉúÎïÐźÅÏìÓ¦ÖµÏÔ×ÅÔöÌí £¬Å¨¶ÈÉý¸ßʱ £¬ÏìÓ¦Öµ·ºÆðïÔÌ­ £¬Òò´Ë £¬×îÖÕÑÜÉú·´Ó¦Ëá¶ÈΪ100g/L ¡£

2.2.3 ÑÇÏõËáįō¶È¶ÔÑÜÉú·´Ó¦µÄÓ°Ïì

׼ȷÎüÊÕµÄ1mlÌðÃÛËØ´¢±¸ÒºÈÜҺƾ֤ÉÏÊöÑÜÉú°ì·¨¾ÙÐÐÑÜÉú»¯ÑÜÉú»¯ £¬ÌðÃÛËØÑÜÉúÎïŨ¶ÈΪ200ug/mL £¬±ùÔ¡·´Ó¦Ìõ¼þÏ £¬¼ÓÈë100g/LµÄÁòËá £¬ºÍ»®·ÖΪ30g/L £¬50g/L £¬70g/L £¬90g/LÑÇÏõËáÄÆ ¡£Ð§¹ûÅú×¢ £¬Ëá¶È´Ó30g/LÖÁ50g/L £¬·´Ó¦ÑÜÉúÎïÐźÅÏìÓ¦ÖµÏÔ×ÅÔöÌí £¬Å¨¶ÈÉý¸ßʱ £¬ÏìÓ¦Öµ·ºÆðïÔÌ­ £¬Òò´Ë £¬×îÖÕÑÇÏõËáÄÆÑÜÉú·´Ó¦Îª50g/L ¡£

3 ʵÑéÊý¾Ý

3.1  ϸÃܶȺÍÖØ¸´ÐÔʵÑé

×¼È·ÒÆÈ¡´¢±¸Òº500uLÓÚÀëÐĹÜÖÐ £¬ÓÃË®¶¨ÈÝ20mLƾ֤ÉÏÊö±êÑùÑÜÉú°ì·¨¾ÙÐÐÑÜÉú»¯ £¬ÑÜÉúÎïŨ¶ÈΪ100ug/mL £¬Æ½ÐÐÖÆ±¸·´Ó¦Òº6´Î £¬ÓÃGC-MS²â¶¨ ¡ £¿¼²ìÑÜÉúÒªÁìµÄÖØÏÖÐÔÒÔ¼°×é·Ö±£´æÊ±¼äºÍ·åÃæ»ýµÄÏà¶Ô±ê×¼Îó²î £¬6¸öƽÐÐÑùµÄÆ× ¡£Ð§¹ûÅú×¢ £¬±£´æÊ±¼äRSDΪ0.98% £¬·åÃæ»ýRSDΪ6.00%, £¬ÏêϸʵÑéÊý¾ÝÈçϱí1Ëùʾ  ¡£

±í1¡¢Öظ´ÐÔ²âÊÔЧ¹û

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

׼ȷÎüÊÕŨ¶ÈΪ10ug/mLµÄÌðÃÛËØ±ê×¼ÈÜÒº10ulÓÚ50mlÀëÐĹÜÖжÔÓ¦ÑÜÉúÎïŨ¶È»®·ÖΪ2ug/mL¡¢10ug/mL¡¢20ug/mL¡¢100ug/mL¡¢200ug/mL £¬Æ¾Ö¤ÉÏÊö±êÑùÑÜÉú»¯°ì·¨¾ÙÐÐÑÜÉú»¯ £¬¾ÙÐÐÏßÐÔ²âÊÔ ¡£ÊµÑéËùµÃÏßÐÔ·½³ÌΪ£ºy=940.43x-3525.57 £¬ÏßÐÔÏà¹ØÏµÊýΪ0.9984 £¬Èçͼ5Ëùʾ ¡£

ΤµÂ1946¡¤(ÖйúÇø)¹Ù·½ÍøÕ¾

ͼ5. ÏßÐÔ¹ØÏµÍ¼

Figure 5 £¬Linear

3.3 ½ÓÄÉÂʲâÊÔ

Ñ¡Ôñ2mg/kg¡¢50mg/kg¡¢200mg/kgµÄ±êÑùÌí¼ÓŨ¶È £¬¶ÔÄ³Æ·ÅÆ°×¾Æ¾ÙÐнÓÄÉÂÊʵÑé £¬Ã¿¸öŨ¶È»®·Ö×öÈý´ÎƽÐÐÑù £¬°´´¦Öóͷ£ÑùÆ·µÄÒªÁì´¦Öóͷ£¼Ó±êºóµÄÑùÆ·²¢²âÊÔ £¬½ÓÄÉÍâ±ê·¨¶¨Á¿ £¬²âÊÔЧ¹ûÈçϱí2Ëùʾ ¡£

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¡¢½ÓÄÉÂʲâÊÔЧ¹û

Table 2, the recovery test results

3.4 ÏÖʵÑùÆ·²âÊÔ

ƾ֤ÉÏÊöÑùÆ·´¦Öóͷ£ÒªÁì¶Ô²î±ðÆ·ÀàµÄ°×¾ÆÑùÆ·¾ÙÐÐǰ´¦Öóͷ£ºÍÑÜÉú»¯ £¬Ê¹ÓÃGC-MS6800¾ÙÐвâÊÔ £¬²âÊÔЧ¹ûÈçϱí3Ëùʾ£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¿²âÊÔЧ¹û

 4 ½áÂÛ

±¾ÊµÑé½ÓÄÉGCMS-6800 £¬ÔÚSIMɨÃèģʽ϶ԾÆÖеÄÌðÃÛËØ¾ÙÐвâÊÔºÍÆÊÎö £¬ÒªÁìÎȹ̿ɿ¿ £¬ÏßÐÔ¹æÄ£ºÃ £¬Ñ¸Ëٶȸß £¬ÊÜÔÓÖÊ·åµÄ×ÌÈÅС £¬Äܹ»ÓÐÓõضԾÆÖеÄÌðÃÛËØ¾ÙÐж¨ÐÔ¶¨Á¿ÆÊÎö ¡£


Ïà¹Ø²úÆ·

ÁªÏµÎ°µÂ¹ú¼Ê1946¹Ù·½Íø

Ïàʶ¸ü¶àÏêϸÐÅÏ¢ £¬ÇëÖµç
400-7102-888
·ÇÊÂÇéʱ¼ä·þÎñÈÈÏß
139 1323 1381
¸øÎÒÃÇÁôÑÔ
ÔÚÏßÁôÑÔ
΢ÐÅÊÛºó·þÎñ¶þάÂë

ÍøÕ¾µØÍ¼