HPLC ·¨¼ì²簇¬¼ÁÖÐÆÏÌÑÌÇË瞋ÇÌ嶹ĺ¬Á¿ 秦瑜丽 (ɽÎ÷Õñ¶«ÖÆÒ©¹É·ÝÓÐÏÞ¹«Ë¾ £¬ ɽÎ÷³¤ÖÎ 047100) 햪튪 [目的 ] 建立测定保健食品片剂中葡萄糖酸亚铁含量的高效液相色谱法 。[ 方法 ]色谱条件为: Agilent ZORBAX SB-C 18 柱( 4. 6 × 150 mm, 5 μm); 以乙腈 - 离子对溶液( 500 ml 纯化水中加四丁基氢氧化铵 10 ml,用磷酸调 pH 至 7. 6) 30∶ 70( V/V)作为流动相; 流速为 1 ml / min; 进样量 20 μl, 检测器在波长 210 nm 处进行检测 。[ 结果 ] 试验表明, 该方法标准曲线良好,线性范围为 62. 5 ~ 625. 0 μg/ml, 回归 方程为 Y =0. 009 2X -0. 116 6, R 2 =0. 999( n =6) 。出峰时间为 1. 547 min, 平均回收率为 96. 68% , RSD 为 1. 5% ( n =6 ) 。[ 结论]该方法 操作简单, 样品前处理简便,结果稳定、 精确, 可用于保健食品片剂中葡萄糖酸亚铁含量的测定。 맘볼듊 高效液相色谱法; 葡萄糖酸亚铁; 片剂; 含量测定 훐춼럖샠뫅 S 609. 9 컄쿗뇪쪶싫 A 컄헂뇠뫅 0517 - 6611( 2013) 08 - 03635 - 02 DEtErmination of FErrous GluconatE in TablEts by HPLC QIN Yu-li ( Shanxi Zhendong PharmaceUtical Co. Ltd, Changzhi, Shanxi 047100) Abstract [ Objective ]To establish a method for the determination of ferroUs glUconate in health food tablets by HPLC. [ Method ]The samples were separated on Agilent ZORBAX SB-C 18 colUmn( 4. 6 × 150 mm, 5 μm) , elUted with mixtUre of acetonitrile and the ion-pairing reagent ( 500 ml of pUrified water added tetra bUtyl ammoniUm hydroxide 10 ml, adjUsted pH to 7. 6 with phosphoric acid)( 30∶ 70, V/V) at 1ml / min. The in- jection volUme Used was 20 μl and the detector wavelength was set at 210 nm. [ ResUlt ]FerroUs glUconate was good linear over the range 62. 5 - 625. 0 μg/ml ( Y =0. 009 2X -0. 116 6, R 2 = 0. 999, n =6) . The peak time was 1. 547 min. The average recovery rate for ferroUs glUconate was 96. 68% , and RSD was 1. 5% ( n =6) . [ ConclUsion ]This method was simple, stable, precise and accUrate. So this stUdy can be Used in determination of ferroUs glUconate content in health food tables. KEy words HPLC; FerroUs glUconate; Tablets; Content determination ퟷ헟볲뷩 秦瑜丽( 1987 - ) , 女, 山西长治人,高级检验工, 从事保健食 品的研发, E-mail: 514016041@ qq. com。 쫕룥죕웚 2013-03-08 ÆÏÌÑÌÇË瞋ÇÌ摠dz£ÓõIJ¹Ì晗ƼÁÖ®Ò» £¬ Ëüº¬ÌúÁ¿½ÏµÍ £¬ ¸±×÷ÓýÏÇá £¬ Ò×ÓÚÎüÊÕ £¬ ¶Ô³¦Î¸µÄ´Ì¼¤Ð¡ 。ÔÚ±£½¡Ê³Æ·ÖÐ £¬ Ëä È»ËùÓмÛλµÄÌú¶¼ÊÇÓÐЧ³É·Ö £¬ µ«ÊÇ Fe 2+ ÖÊÁ¿¸üÓÅ 。《 Öйú Ò©µä 》 ²ÉÓõζ¨·¨²â¶¨ÆÏÌÑÌÇËáÑÇÌúº¬Á¿ £Û 1 £Ý £¬ µ«ÊÇ´Ë·½·¨Ñù Æ·Ç°´¦Àí·±Ëö £¬ ²Ù×÷¸´ÔÓ £¬ ÈËΪÎó²î½Ï´ó £¬ ²¢ÇÒÖ»Äܲ箏Ã×Ü Fe 2+ µÄÁ¿ £¬ ¶ø²»Äܲ筝¨ÆÏÌÑÌÇËáÑÇÌúµÄº¬Á¿ 。±ÊÕßÔڲο¼Ïà ¹ØÎÄÏ× £Û 2-4 £Ý µÄ»ù´¡ÉϽ蘯ϲúÆ·µÄÌص㠣¬ È·¶¨Àë×Ó¶ÔÊÔ¼ÁµÄÖÖ À犲ÍÌ晴ÓÁ¿ÒÔ¼° pH µÄ·¶Î§ £¬ È·±£ÎÞÌØÕ÷ÎüÊÕ·蠏ÄÆÏÌÑÌÇËá ÑÇÌ昤ڹ̶¨Ï猖ϵı£Áôʱ¼äºÍ·衵δó´ó¸ÄÉÆ 。½á¹ûÖ¤Ã÷ £¬ ¸Ã ·½·¨Îȶ¨ÐÔºÍÖظ´ÐԺà £¬ ÁéÃô¶È¸ß £¬ ¿ÉÓÃÓÚÆÏÌÑÌÇË瞋ÇÌ惕à ±£½¡Ê³Æ·µÄÖÊÁ¿¿ØÖÆ 。 1 닄쇏폫랽램 1. 1 닄쇏 Ö÷ÒªÊÔ¼Á :ÆÏÌÑÌÇË瞋ÇÌ巐ÔÕÕÆ· £¬ Ö£ÖÝÈðÆÕÉúÎï ¹¤³ÌÓÐÏÞ¹«Ë¾ ;±£½¡Ê³Æ·Æ¬¼Á £¬ ɽÎ÷Õñ¶«ÖÆÒ©¹É·ÝÓÐÏÞ¹«Ë¾ Ñз¢²¿ ;ËĶ¡»ùÇ簷õ»¯ï§ ( 10% ) £¬ Ìì½òÊй篋´¾«Ï¸»¯¹¤Ñо¿ Ëù£¬ ·ÖÎö´¿ ;Á×Ëá £¬ ±±¾©»¯¹¤³§ £¬ ·ÖÎö´¿ ;ÒÒëæ £¬ ÃÀ¹úÌìµØÊÔ¼Á ¹«Ë¾ £¬ É«Æ×´¿ ;ÁÚ¶þµª·Æ £¬ Ìì½òÊпÆÃÜÅ·»¯Ñ§ÊÔ¼ÁÓÐÏÞ¹«Ë¾ £¬ ·ÖÎö´¿ ;ÁòËá £¬ Â衽ôÊл¯Ñ§ÊÔ¼Á³§ £¬ ·ÖÎö´¿ ;п·Û £¬ Ìì½òÊй⸴ ¾«Ï¸»¯¹¤Ñо¿Ëù ;ÊÔÑéÓÃË®¾ùΪ´¿»¯Ë® 。Ö÷ÒªÒÇÆ÷ : UitlMate 3000 ¸ßЧҺÏàÉ«Æ×ÒÇ 、 ×ÏÍâ¼ì²âÆ÷ 、 ±ê×¼×Ô¶¯½øÑùÆ÷ 、 ÖùΠÏä 、 pH ¼Æ ( UB-7) 、 T-214 ÐÍ΢Á¿·ÖÎöÌìƽ £¬ ±±¾©Èü¶狢鉧¹ÒÇÆ÷ ϵͳÓÐÏÞ¹«Ë¾ 。 1. 2 랽램 1. 2. 1 HPLC ·¨ 。 1. 2. 1. 1 Á÷¶¯ÏàµÄÅäÖÆ 。1 000 ml ´¿»¯Ë®ÖмÓËĶ¡»ùÇ簷õ »¯ï§ ( 10% ) 20 ml£¬ ÓÃÁ×Ë盞÷ pH ÖÁ 7. 6£¬ ÓëÒÒë豌´ 70∶ 30 »ìºÏ ¾ùÔÈ £¬ ¹ý 0. 45 μm µÄĤ £¬ ³¬Éù 30 min£¬ ±¸Óà 。 1. 2. 1. 2 ±ê×¼ÈÜÒºµÄÖƱ¸ 。¾«ÃܳÆÈ¡ÆÏÌÑÌÇË瞋ÇÌ巐 0. 012 5 g£¬ Öà 50 ml ×ØÉ«ÈÝÁ¿Æ¿ÖÐ £¬ ¼ÓÁ÷¶¯Ï猜ܽ筝¨ÈÝ £¬ ³¬Éù 20 min£¬ ¹ý 0. 45 μm ÂËÍ· £¬ ÔÙ³¬Éù 10 min£¬ µÃ 250 μg / ml ¶ÔÕÕ Æ·ÈÜÒº 。ͬ·¨ÔÙ·Ö±ðÅ葷ÆŨ¶ÈΪ 0、 62. 5、 125. 0、 187. 5、 250. 0、 375. 0、 625. 0 μg/ ml µÄÆÏÌÑÌÇË瞋ÇÌ昕µÁбê× Òº £¬ ´ýÓà 。 1. 2. 1. 3 ÒõÐÔ¶ÔÕÕÈÜÒºµÄÖƱ¸ 。°´±£½¡Ê³Æ·´¦·½³ÆÈ ÌÑÌÇË瞋ÇÌ昮ÔÍ箏ÄÆ萢鋕¸¨ÁÏ 0. 014 0 g£¬ Öà 50 ml ×ØÉ«ÈÝÁ¿ Æ¿ÖÐ £¬ ¼ÓÁ÷¶¯Ï猜ܽ筝¨ÈÝ £¬ ³¬Éù 20 min£¬ ¹ý 0. 45 μm ÂËÍ· £¬ ÔÙ ³¬Éù 10 min£¬ µÃÒõÐÔ¶ÔÕÕÈÜÒº £¬ ´ýÓà 。 1. 2. 1. 4 ¹©ÊÔÆ·ÈÜÒºµÄÖƱ¸ 。È¡±£½¡Ê³Æ·Æ¬¼Á 50 Ƭ £¬ ¾«ÃÜ ³ÆÖØ £¬ ³ýÈ¥°üÒ £¬ ÑÐϸ £¬ ¾«ÃܳÆÈ¡ 0. 028 8 g Öà 50 ml ×ØÉ«ÈÝÁ¿ Æ¿ÖÐ £¬ ¼ÓÁ÷¶¯Ï猜ܽ筝¨ÈÝ £¬ ³¬Éù 20 min£¬ ¹ý 0. 45 μm ÂËÍ· £¬ ÔÙ ³¬Éù 10 min£¬ ´ýÓà 。 1. 2. 1. 5 ϵͳÊÊÓ¦ÐÔÊÔÑé 。¾«ÃÜÁ¿È¡ “ 1. 2. 1. 2 ” Ïî϶ÔÕÕ Æ·ÈÜÒººÍ “ 1. 2. 1. 3” Ï隝ÂÒõÐÔ¶ÔÕÕÈÜÒº¸÷ 20 μl£¬ ½øÑùºó¼Ç¼ É«Æ×ͼ 。 1. 2. 1. 6 ÏßÐÔ¹Øϵ¿¼²ì 。½« “ 1. 2. 1. 2” ÏîÏÂϵÁбê×¼ÈÜ °´ÒºÏ猯õ¼þ²筝¨ £¬ ÒÔÆÏÌÑÌÇË瞋ÇÌ愰¨¶ÈΪº瞹ø±ê £¬ ÒÔ·åÃæ»ý Ϊ×Ý×ø±ê £¬ »贍Ʊê×¼Ç昕ß 。 1. 2. 2 µÎ¶¨·¨ 。È¡ÑùÆ· 50 Ƭ £¬ ¾«Ãܳƶ¨ £¬ ÑÐϸ £¬ ¹ý 40 Ŀɸ £¬ »ìºÏ¾ùÔÈ 。³ÆÈ¡¾ùÔÈÑùÆ· 4. 186 0 g£¬ ÖÃÓÚ¾ßÈû׶ÐÎÆ¿ÖÐ £¬ ¼Ó ÈëË® 75 ml Óë 1 mol/L ÁòËáÈÜÒº 15 ml£¬ Èܽâºó £¬ ¼Óп·Û 0. 75 g£¬ ÃÜÈû £¬ ·ÅÖÃÔ¼ 20 min£¬ Ö±ÖÁÈÜÒºÍÑÉ« 。ÓÃÆÌÓÐп·ÛµÄ 4 ºÅ´¹ ÈÛ©¶·Â˹ý £¬ ÂËÆ÷ÓÃззÅÀ莊ÄË® 20 ml Ï´µÓ £¬ ºÏ²¢Ï´ÒºÓëÂË Æ÷ £¬ ¼ÓÁÚ¶þµª·ÆָʾҺ 0.2 ml£¬ ÓÃÁòËá鮻µÎ¶¨Òº ( 0.1 mol/L) µÎ¶¨ÖÁÈÜÒºÓÉéÙ»Æɫת±萸ªÂÌÉ« £¬ ²¢½«µÎ¶¨µÄ½盪﨧ÿհ 낲믕얩튵뿆톧ꎬ JoUrnal of AnhUi Agri. Sci. 2013ꎬ 41⠩⁔樍 8⤩ⴲ㠴⠺⥝⁔䨍 3635 - 3636 퓰죎뇠벭 李菲菲 퓰죎킣뛔 卢瑶