TP CH KHOA HC, i hc Hu, Tp 74B, S 5, (2012), 185-191

PHN TCH V NH GI HM LNG NITRAT, NITRIT TRONG MT S THC PHM CH BIN LU HNH THNH PH HU L Th Kim Tin1, Nguyn Vn Ly2
1

Trng i hc S phm, i hc Hu
2

Trng i hc Khoa hc, i hc Hu

Tm tt. Xc xch, lp xng, tht xng khi l cc loi thc phm ch bin c ngi dn tiu th vi s lng ln. V v y, vic phn tch hm lng nitrat, nitrit c trong cc loi thc phm tr nn v cng quan trng. Kt qu phn tch bng phng php quang ph hp th phn t UV- VIS cho thy hm lng nitrat, nitrat trong ba loi thc phm ch bin ni trn nm trong gii hn cho php theo Quyt nh s 867/1998/Q-BYT ca B Y t.

1. M u Thc phm l nhu cu thit yu ca con ngi. N cung cp nng lng, cht dinh dng cho con ngi lao ng, pht trin v duy tr s sng. Tuy nhin nu chng ta s dng thc phm khng m bo v sinh an ton th s dn n s ng c, tc h i khng tt cho sc khe. Mt trong nhng nguyn nhn gy nn ng c l s dng cc ha cht trong vic ch bin, bo qun khng ng quy nh v liu lng vt qu tiu chun cho php [6]. X hi ngy cng vn minh, tin b th con ngi cng phi i u nhiu hn vi him ha ha cht c s dng trong thc phm. Do , ngy nay vn ha cht trong thc phm vn ang l mi lo ngi ca tt c chng ta. Trong s cc ha cht m ngi ta dng bo qun thc phm th mui nitrat v mui nitrit c s dng ph bin. Trn th trng bn loi mui thng c s dng l: natri nitrat, natri nitrit, kali nitrat v kali nitrit [7]. y l bn loi mui c xp vo nhm cht bo qun c chc nng n nh mu, c dng trong phomat, cc loi tht, nc gii kht, thy sn ch bin. Cc mui ny c hai cng dng: to mu cho c v tht, ng thi ngn chn s pht trin ca mt loi vi khun gy ng c tht. Vi cng dng nh vy, ngi sn xut khng ngn ngi a cc mui ny vo thc phm. Nhng mt s t h khng h bit r tc hi ca nhng loi mui ny nu hm lng vt qu tiu chun cho php. Mui nitrat (NO3-) khi vo c th ngi tham gia phn ng kh d dy v ng rut do tc dng ca cc men tiu ha sinh ra NO2 - [8]. Nitrit sinh ra phn ng
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Phn tch v nh gi hm lng nitrat

vi Hemoglobin to thnh methemoglobin lm mt kh nng vn chuyn oxi ca Hemoglobin. Thng thng Hemoglobin cha Fe2+, ion ny c kh nng lin kt vi oxi. Khi c mt NO2- n s chuyn ha Fe2+ lm cho hng cu khng lm c nhim v chuyn ti O2. Nu duy tr lu s dn ti t vong. 2HbFe2+(O2) + NO2- + H2O 2HbFe3+ + 2OH- + NO3- + O2 S to thnh methemoglobin c bit thy r tr em. Tr em mc chng bnh ny thng xanh xao v d b e da n cuc sng c bit l tr di 6 thng tui. Ngoi ra, NO2- trong c th d tc dng vi cc amin to thnh nitrosamine- mt hp cht tin ung th [8]. Do tc hi ca NO3- , NO2- n con ngi nh vy nn vic xc nh hm lng nitrat, nitrit trong cc loi thc phm l rt cn thit nhm m bo s an ton cho ngi tiu dng. Thnh ph Hu l ni tp trung dn c ng c ca tnh Tha Thin Hu. Ni y lng thc phm ch bin c nhp vo v tiu th vi lng ln, nn vic kim tra cht lng v sinh an ton thc phm cng tr nn quan trng. Trong bi bo ny chng ti trnh by kt qu phn tch hm lung nitrat, nitrit trong mt s thc phm ch bin lu hnh thnh ph Hu bng phng php quang ph hp th phn t UV- VIS trn c s phn ng to hp cht mu azo ca nitrit v i axit sunfanilic v -naphtylamin. 2. Nguyn liu v phng php thc nghim 2.1. Thit b, dng c, ha cht 2.1.1. Thit b, dng c My trc quang UV-VIS: T80+ UV/VIS Spectrometer, M sn xut.; My o pH: 330 i/SET, c sn xut; Cn phn tch, my rung siu m; My nc ct hai ln: Fistreem Cyclon, Anh sn xut; Cc dng c thy tinh: bnh nh mc, cc m, pipet, buret, a thy tinh,... bnh tia, bp cao su,... 2.1.2. Ha cht Hu ht cc ha cht c xut x Trung Quc bao gm: SA, NA, HCl, EDTA, NH4Cl, K4[Fe(CN)6], Na2B4O7.5H2O, Zn(CH3COO)2, Cd, KNO3, KNO2. Dung dch gc KNO3 1,0 g/L c pha bng cch: Ha tan 0,50 g KNO3 trong nc, bo qun vi 1 mL chloroform, nh mc thnh 500 mL. Dung dch trung gian KNO3 0,1 g/L : Pha long 10,0 mL dung dch gc thnh 100 mL bng nc ct. Dung dch lm vic KNO3 10 mg/L : Pha long 10,0 mL dung dch trung gian thnh 100 mL bng nc ct. Dung dch gc KNO2 1,0 g/L : Ha tan 0,50 g KNO2 trong nc, bo qun vi 1mL chloroform, nh mc thnh 500 mL. Dung dch trung gian KNO2 0,1 g/L : Pha long 10,0 mL dung dch gc thnh 100 mL bng nc ct.

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2.2. Ly mu v x l mu y, cc i tng nghin cu: Xc xch, lp xng, tht xng khi, u c thng hiu nn c th ly bt k a im no lm mu i din. Cc mu thc ph m c chng ti ly ti siu th Big C; t thng 4 n thng 7 nm 2012, tn sut 3 lo i mu / 1 thng theo nh k sn xut ca hng ch bin cc loi mu trn. Cc mu sau khi ly v c bo qun theo cc iu kin ghi trn bao b. Trc khi tin hnh xc nh hm lng nitrat, nitrit, cc mu thc phm ch bin c xay nh v x l theo phng php ngm chit [3], [4], [5]. 2.3. Phng php phn tch Trong ti ny, phn tch hm lng nitrat, nitrit trong thc phm ch bin, chng ti chn phng php quang ph hp th phn t UV- Vis trn c s phn ng to hp cht mu azo ca nitrit vi axit sunfanilic v -naphtylamin [1], [2]. 2.4. Phng php nh gi kt qu phn tch Cc kt qu phn tch c tin cy c nh gi thng qua cc i lng nh RSD%, RSDH, nu RSD% 0,5 RSDH th phng php c lp li tt, tin cy cao [3]. Ngoi ra kt qu c nh gi da vo Quyt nh s 867/1998/Q-BYT ca B Y t [8]. 3. Kt qu v tho lun 3.1. Kho st cc iu kin thch hp v xy dng qui trnh phn tch hp th quang ca hp cht mu azo ph thuc vo cc yu t: bc sng, thi gian n nh mu, mi trng pH, t l nng SA/NA. Sau y l cc iu ki n thch hp c kho st xc nh nitrat, nitrit. Thi gian n nh mu: t 15-30 pht Mi trng: pH 2

T l nng SA/NA: CSA/NA = 1 vi CSA = CSA = 2,5.10-4 M. kh t nitrat qua nitrit, chng ti tin hnh kho st hai phng php: Kh bng hn hp dung dch CdSO4 - Huyn ph Zn v kh bng ct kh Cd-Cu [3],[4]. Kt qu kho st cho thy phng php kh bng ct kh Cd-Cu cho hiu sut kh tt hn vi cc iu kin kh c chn nh sau: Mi trng kh: pH 8,5 s dng hn hp NH4Cl EDTA Tc chy qua ct: 6 mL/pht T cc kt qu kho st trn chng ti xy dng ng chun xc nh nitrat, nitrit, qua c th xc nh c gii hn pht hin v gii hn nh lng ca phng php. Kt qu nh gi s mt mt ca nitrit qua qu trnh x l mu khng ng k.

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Trn c s cc iu kin thch hp v phng php kho st, chng ti xy dng c qui trnh phn tch hm lng nitrat, nitrit trong thc phm ch bin nh sau: Mu thc phm c xay nh, cn 30g mu thm 100 mL nc ct nng, 8mL natri borat bo ha, 0,5g than hot tnh; ngm chit 60-700C khong 15 pht; ngu i n nhit phng; thm 5mL K4[Fe(CN)6] 0,4 M; 5mL Zn(CH3COO)2 10%, 8mL natri borat bo ha; m i ln thm ha cht cn yn 20-30 pht. Sau nh mc n 250mL, lng 30 pht. Lc ly dch lc. + Xc nh nitrit: Ly 10 mL dung dch mu (V1) thm chun bng KNO2 10 mg/L , 0,2mL HCl 0,16M, 1mL EDTA 0,013M, 5mL SA 0,0025M, 0,5mL NA 0,025M; nh mc n 50 mL (V2); sau 15 pht o quang. Hm lng nitrit c tnh theo cng thc:
(*)

) + Xc nh tng hm lng nitrat, nitrit: Ly 10 mL dung dch mu (V3) thm chun bng KNO3 10 mg/L; 2mL hn hp EDTA NH4Cl, nc ct, c th tch sau khi qua ct l 20 mL (V4). Ly 10mL (V5) dung dch sau khi qua ct thm vo 0,2mL HCl 0,16 M, 5mL SA 0,0025M, 0,5 mL NA 0,025M; nh mc thnh 50mL (V6), sau 15 pht o quang. Hm lng tng nitrat, nitrit c tnh theo cng thc:

Hm lng nitrat:

Trong : a l h s chn v b l h s gc trong phng trnh ng thm chun xc nh nitrat, nitrit. 3.2. Kt qu phn tch hm lng nitrat, nitrit trn cc mu thc phm ch bin
Bng 3.1. Kt qu phn tch trn mu Xc xch b Vissan

t ly mu Hm lng (mg/kg) Kali nitrit

Ngy ly mu 05/06/2012 (NSX 09/05/12 HSD 09/08/12) 3,784 0,006 (n=3)

Ngy ly mu 21/06/2012 (NSX 05/06/12 HSD 05/09/12) 1,30 0,012 (n=3)

Ngy ly mu 10/07/2012 (NSX 26/06/12 HSD 26/09/12) 2,275 0,007 (n=3)

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RSD = 0,159 0,5.RSDH = 0,81 Kali nitrat 19,686 0,033 (n=3) RSD = 0,17 0,5.RSDH = 0,64 65,5 0,1 %

RSD = 0,923 0,5.RSDH = 0,96 22,39 0,12 (n=3) RSD = 0,507 0,5.RSDH= 0,621 61,73 0,01 %

RSD = 0,308 0,5.RSDH = 0,883 20,125 0,095 (n=3) RSD = 0,473 0,5.RSDH = 0,621 64.21 0,01%

Nhn xt: Bng 3.1. cho thy, hm lng trung bnh ca kali nitrat, nitrit qua 3 t ly mu, trong Xc xch b Vissan tuy c sai khc nhau nhng vn di ngng cho php ca B Y t (125 mg KNO2/kg; 250 mg KNO3/kg) [8].
Bng 3.2. Kt qu phn tch trn mu lp xng Vissan

t ly mu Hm lng (mg/kg) Kali nitrit

Ngy ly mu 05/06/2012 (NSX 26/04/12 HSD 26/11/12) 19,2470,072 (n=3) RSD = 0,374 0,5.RSDH=0,641 148,71 0,672 (n=3) RSD = 0,452 0,5.RSD= 0,471 14,39 0,01 %

Ngy ly mu 21/06/2012 (NSX 16/05/12 HSD 16/12/12) 10,853 0,106 (n=3) RSD = 0,977 0,5.RSDH= 1,518 67,7670,336 (n=3) RSD = 0,496 0,5.RSDH= 0,530 10,18 0,01 %

Ngy ly mu 10/07/2012 (NSX 02/06/12 HSD 02/01/13) 17,008 0,048 (n=3) RSD = 0,282 0,5.RSDH = 0,653a 100,3820,413 (n=3) RSD = 0,411 0,5.RSDH = 0,500 12,23 0,00%

Kali nitrat

Nhn xt: Bng 3.2. cho thy, hm lng kali nitrat, nitrit trung bnh qua 3 ln ly mu trong lp xng Vissan c sai khc nhau v cao hn trong xc xch nhng v n di ngng cho php ca B Y t (125 mg KNO2/kg; 250 mg KNO3/kg).
Bng 3.3. Kt qu phn tch trn mu tht ba ri xng khi Le Gourmet

t ly mu Hm lng (mg/kg) Kali nitrit

Ngy ly mu 25/06/2012 (NSX 19/06/12 HSD 28/07/12) 1,834 0,012 (n=3) RSD = 0,654

Ngy ly mu 10/07/2012 (NSX 29/06/12 HSD 07/08/12) 2,315 0,006 (n=3) RSD = 0,259

Ngy ly mu 20/07/2012 (NSX 08/07/12 HSD 16/08/12) 2,853 0,006 (n=3) RSD = 0,210

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0,5.RSDH=0,913 Kali nitrat 21,986 0,123 (n=3) RSD= 0,558 0,5.RSDH=0,628 55,06 + 0,01%

0,5.RSDH =0,881 22,415 0,102 (n=3) RSD = 0,453 0,5.RSDH =0,626 42,04 + 0,00%

0,5.RSDH = 0,854 21,297 0,061 (n=3) RSD = 0,286 0,5.RSDH = 0,631 42,04 + 0,00%

Nhn xt: Bng 3.3. cho thy, hm lng trung bnh ca kali nitrat, nitrit trong tht ba ri xng khi Le Gourmet qua 3 ln ly mu c sai khc nhau nhng vn di ngng cho php ca B Y t (125 mgKNO2/kg; 250 mgKNO3/kg). 4. Kt lun nghin cu tm ra cc iu kin thch hp cho phng php v xy dng quy trnh phn tch xc nh hm lng nitrat, nitrit bng phng php trc quang. Kt qu cho thy phng php c tin cy tt, c th p dng cho vic xc inh hm lng nitrat, nitrit trong cc mu thc phm ch bin. p dng phng php xc nh c hm lng nitrat, nitrit trong ba loi mu thc phm ch bin: xc xch, lp xng, tht xng khi lu hnh ti Hu trong thi gian t thng 4 n thng 7/2012. Kt qu cho thy, cc thc phm c phn tch tuy c hm lng nitrat, nitrit khc nhau ng k nhng vn nm trong gii hn cho php ca B Y t quy nh. TI LIU THAM KHO
[1]. B Y t, Danh mc tiu chun v sinh i vi lng thc, thc phm, Quyt nh s 867/1998/Q-BYT, 1998. [2]. Tiu chun Vit Nam 6839, Sa bt- xc nh hm lng nitrat v nitrit- phng php kh bng cadimi v o ph, B Khoa hc cng ngh v mi trng, H Ni, 2001. [3]. Miller J. C. and Miller J. N., Statistics for analytical chemistry, Ellis Horwood Limited, Great Britain, 1988. [4]. R. Michalski, I. Kurzyca, Determination of Nitrogen Species (Nitrate, Nitrite and Ammonia Ions) in Environmental Samples by Ion Chromatography, Polish Journal of Environmental Studies Vol. 15, No. 1 (2006), 5-18. [5]. Man- fung, Samuel, Briefing session on analysis of nitrate/nitrite and propionic acid in food, Government laboratory HKSARG, 2008. [6]. http://docx.vn/tai-lieu/28480/Nitrates---Nitrits-trong-thuc-pham.tailieu [7]. http://community.h2vn.com/index.php?topic=13831.0 [8]. http://www.scribd.com/doc/55348868/Nitrat-Nitrit-daihoc-com-Vn

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AN ANALYSIS AND EVALUATION FOR NITRATE, NITRITE CONTENTS IN SOME KINDS OF PROCESSED FOOD CIRCULATED IN HUE CITY Le Thi Kim Tien1, Nguyen Van Ly2
1

College of Education, Hue University

2

College of Sciences, Hue University

Abstract. Sausage, Chinese sausage, Smoked bacon are kinds of processed food consumed in large quantity. As a result, the analysis of nitrate, nitrite contents in those kinds of food becomes crucial. The results of the analysis by Ultraviolet Visible Spectrometry show that the nitrate and nitrite contents in three aforementioned types of food are in the permitted limits according to the decision number 867/1998/Q-BYT of Ministry of Medicine.