CN104267153A - Cigarette smoke acidity index evaluation model establishment method based on gustation vitality values - Google Patents

Cigarette smoke acidity index evaluation model establishment method based on gustation vitality values Download PDF

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CN104267153A
CN104267153A CN201410544976.5A CN201410544976A CN104267153A CN 104267153 A CN104267153 A CN 104267153A CN 201410544976 A CN201410544976 A CN 201410544976A CN 104267153 A CN104267153 A CN 104267153A
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acid
flue gas
sense
main flume
tart flavour
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CN104267153B (en
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冒德寿
李智宇
者为
刘强
付磊
王凯
侯春
洪鎏
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China Tobacco Yunnan Industrial Co Ltd
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Abstract

The invention relates to a cigarette smoke acidity index evaluation model establishment method based on gustation vitality values, and belongs to the technical field of cigarette evaluation. The method comprises the steps as follows: a gas chromatograph-mass spectrometer is utilized to detect the content of organic acids in mainstream cigarette smoke with an N,O- bis(trimethylsilyl)trifluoroacetamide derivatization method; according to a public reported gustation threshold, the gustation vitality values of the organic acids are calculated so as to recognize key acidity substances in the mainstream cigarette smoke; a cigarette smoke acidity index evaluation model is established on the basis of the key acidity substances in the mainstream cigarette smoke; and human sense evaluation of the cigarette smoke acidity intensity is performed by a cigarette sense technician, and statistical software is adopted to perform fitting effect analysis on the cigarette smoke acidity index and a human sense evaluation value. The cigarette smoke acidity index evaluation model and a human sense evaluation method have an ideal fitting effect, the cigarette smoke acidity intensity is objectively evaluated, and the method can be used for development of the cigarette product flavor technology.

Description

Based on the flue gas tart flavour index assessment method for establishing model of sense of taste energy value
Technical field
The invention belongs to cigarette evaluation and test technical field, be specifically related to a kind of flue gas tart flavour index assessment method for establishing model based on sense of taste energy value.
Background technology
Cigarette product style and features is the soul of cigarette product, through cigarette product life cycle all the time.The evaluation of tobacco and tobacco product comprises the aspects such as vision, the sense of hearing, sense of smell, the sense of taste and sense of touch, vision is how relevant with appearance factor with hearing evaluation, sense of smell, the sense of taste and sense of touch evaluation are then closely related with style and features, only have the common impression by sense of smell, the sense of taste and sense of touch, could comprehensive, objective, evaluating cigarette product style feature exactly.
Scientific research personnel has carried out a large amount of exploratory development to flue gas aromatic style feature, but is still in the starting stage to the research of flue gas sense of taste style and features evaluation method.Have the special project evaluation for flue gas tart flavour in the Chinese-style cigarette style and features sensory evaluation method set up at present, but it is still smoked panel test based on human body, process difficult of smokeing panel test gets rid of artificial subjectivity and consequent uncertainty.
Natural numerous food product and spices, as Radix Angelicae Sinensis, mango, banana, cucumber and coriander etc., it is not principal ingredient with causing taste composition that its key causes fragrant, micro constitutent often, and its profoundness is that compound is except content height, also has threshold properties.At present, to have developed in many tobacco leaves or flue gas organic acid detection method to obtain organic acid quantitative data, but the effect of these methods and quality or style and features relevance is undesirable.
Now, domestic tobacco business forms material square foundation face in threshold application technological means anatomy quality or style and features and is also in blank; Applying electronic tongue bionics techniques differentiates that flue gas tart flavour, sweet taste, bitter taste and saline taste intensity are emerging a kind of objective quantification characterizing methods, but the method exists testing result is subject to the factor such as artificial saliva, flue gas complex sample contaminant sensor and occurs unstable shortcoming.Chinese-style cigarette the most significantly taste characteristics is tart flavour and sweet taste, setting up a kind of can the objective quantification index assessment model that characterizes flue gas sourness intensity be one of technical field of tobacco technical matters urgently to be resolved hurrily, and this can disclose for flue gas tart flavour characteristic mechanisms and control technique provides and instruct reference.
Summary of the invention
The object of the invention is to the deficiency for existing flue gas tart flavour evaluation method, a kind of flue gas tart flavour index assessment method for establishing model based on sense of taste energy value is provided, desirable fitting effect can be obtained with human body evaluation by the method, realize the objective evaluation of flue gas sourness intensity, for flue gas sense of taste characteristic evaluating and regulation and control provide technical support.
The object of the invention is to be achieved through the following technical solutions:
Flue gas tart flavour index assessment method for establishing model based on sense of taste energy value of the present invention, comprises the steps:
Step (1), the detection of main flume organic acid content: utilize N, two (TMS) trifluoroacetamide (BSTFA) the derivatization method pretreatment technology of O-and gas chromatograph-mass spectrometer realize the quantitative test of organic acid content in main flume, wherein, the Small molecular low boiling molecules such as formic acid, acetic acid and propionic acid easily pass through cambridge filter, main flume total content is represented by gas gas-phase objects and granule phase substance sum, all the other higher boiling molecules are easily retained by cambridge filter, represent main flume total content with granule phase substance;
Step (2), the identification of the crucial sour odour material of main flume: the taste threshold that the main flume organic acid content utilizing step (1) to obtain and document are openly reported, calculates each organic acid sense of taste energy value TAV=main flume organic acid content/taste threshold; When certain organic acid TAV >=0.1, then it is identified as the crucial sour odour material in main flume, otherwise, then ignore;
Step (3), the foundation of flue gas tart flavour index assessment model: in the main flume obtain step (2), crucial sour odour material TAV sues for peace to set up flue gas tart flavour index assessment model, flue gas tart flavour index=each crucial organic acid sense of taste energy value sum;
Step (4), the evaluation of flue gas tart flavour index assessment model: organize cigarette sense organ technician, human body evaluation is carried out to flue gas sourness intensity, and adopts SPSS or Unscrambler statistical software, score value is evaluated to flue gas tart flavour index and human body and carries out fitting effect analysis.
In technical solution of the present invention, main flume described in step (1) is the main flume that flammable suction tobacco and tobacco product produce through burning.
Further, preferably main flume described in step (1) is the main flume that cigarette, cigar, pipe tobacco, redried leaf tobacco, stem or reconstituted tobacoo produce through burning.
In technical solution of the present invention, in main flume, organic acid comprises three classes: formic acid, acetic acid, propionic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid, 3 methylvaleric acid, the VFAs such as caproic acid; Enanthic acid, sad, n-nonanoic acid, capric acid, benzoic acid, phenylacetic acid, oleic acid, linoleic acid, leukotrienes etc. partly volatilize organic acid; Oxalic acid, lactic acid, malic acid, citric acid, succinic acid, lauric acid, myristic acid, palmitic acid, the difficulty such as benzenpropanoic acid volatilization organic acid.
The quantitative analysis method of main flume organic acid utilizes N, two (TMS) trifluoroacetamide (BSTFA) derivatization method of O-completes, concrete grammar see Zhang Yingchun etc., Journal of Analytical Science, 2010, described in 26 (5): 567-571.The Small molecular low boiling molecules such as formic acid, acetic acid and propionic acid are easily by cambridge filter, and represent main flume total content by gas gas-phase objects and granule phase substance sum, all the other higher boiling molecules are easily retained by cambridge filter, represent main flume total content with granule phase substance.Gas chromatograph-mass spectrometer mass analyzer used is any one of commercially available quadrupole rod mass analyzer, ion strap mass analyzer and time of flight mass analyzer, without particular/special requirement.
The checking of described flue gas tart flavour index assessment model, organize 11-23 name cigarette sense organ technician, human body evaluation is carried out to flue gas sourness intensity, and adopts SPSS or Unscrambler statistical software, score value is evaluated to flue gas tart flavour index and human body and carries out fitting effect analysis.
The present invention compared with prior art, its beneficial effect is: the invention provides a kind of flue gas tart flavour index assessment model set up based on sense of taste energy value, objective quantification can characterize flue gas sourness intensity, and achieve desirable fitting effect with human body evaluation assessment, solve in sensory evaluation flue gas sourness intensity process by the problem that artificial subjectivity and consequent uncertainty etc. affect; The present invention can be used for the exploitation of the announcement of flue gas tart flavour characteristic mechanisms and flavoring technology.
Accompanying drawing explanation
Fig. 1 is the correlation test figure that exponential model method of the present invention and sensory evaluation method are evaluated 51 parts of flue gas sample tart flavours.
Embodiment
Below in conjunction with the present invention will be further described by reference to the accompanying drawings.
Reagent required for the present invention, material and instrument:
11 raw tobacco material main producing regions such as Yunnan, Fujian, Guizhou, Hunan, Jiangxi, Sichuan, Heilungkiang, Hubei, Brazil, the U.S. and Zimbabwe amount to 51 parts of tobacco leaf samples, wherein, and burley tobacco leaf 5 parts, 1 part, suncured tabacco, stem 1 part, flue-cured tobacco 44 parts; Upper tobacco leaf 25 parts, 18 parts, middle part tobacco leaf, lower tobacco leaf 8 parts; 9 parts, external tobacco leaf, wherein, 3 parts, Zimbabwe, Brazil 4 parts, 2 parts, U.S., 42 parts, domestic tobacco leaf.
Cigarette is rolled by GB 5606 3-1996 method, more than 48h is balanced under being positioned over temperature 22 ± 1 DEG C, relative humidity 60 ± 3% environment, select cigarette within the scope of average quality ± 0.020g and average resistance to suction ± 49Pa for experiment cigarette, detect for flue gas organic acid and the sensory evaluation of tart flavour.
Methyl alcohol and methylene chloride are chromatographically pure traditional Chinese medicines reagent company limited;
Formic acid (33015, >=98%), acetic acid (320099, >=99.7%), propionic acid (402907, >=99.5%), isobutyric acid (58360, >=99.5%), butyric acid (B103500, >=99%), isovaleric acid (129542, >=99%), valeric acid (V0125, >=99%), 3 methylvaleric acid (222453, >=97%), caproic acid (153745, >=99.5%), enanthic acid (75190, >=99%), sad (C2875, >=99%), n-nonanoic acid (N5502 >=97%), capric acid (C1875 >=98%), benzoic acid (242381, >=99.5%), phenylacetic acid (78490, >=98%), benzenpropanoic acid (P16001, >=99%), palmitic acid (P0500, >=99%), oleic acid (O1008, >=99%), oxalic acid (75688, >=99%), lactic acid (69785, >=90%), malic acid (240176. >=97%), citric acid (251275, >=99.5%), succinic acid (S3674, >=99%), trans-2-hexenoic acid (193089, >=99%), two (trimethyl silicon based) trifluoroacetamide (155195, >=99%) of N, O-and trans-cinnamic acid (C80857, >=99%) all derive from Sigma-Aldrich company.All samples is all kept at lower than for subsequent use in 4 DEG C of refrigerators.
The semi-automatic 20 duct smoking machines of RM20H, German Borgwaldt company;
Gas chromatograph-mass spectrometer, Aglient 7890GC/5973MS;
Jy92-2D ultrasonic cell disrupte instrument, NingBo XinZhi Biology Science Co., Ltd;
F319-04 cambridge filter, Whatman Inc. (US);
Agilent 1100 high performance liquid chromatograph, AE163 electronic balance, sensibility reciprocal 0.1mg, Mei Teletuo benefit company of Switzerland.
Based on the flue gas tart flavour index assessment method for establishing model of sense of taste energy value, comprise the steps:
Step (1), the detection of main flume organic acid content: utilize N, two (TMS) trifluoroacetamide (BSTFA) derivatization method of O-completes, see Zhang Yingchun etc., Journal of Analytical Science, 2010, described in 26 (5): 567-571.Concrete grammar is as follows: cambridge filter is loaded flue gas supplementary set device, by the Cigarette that YC/T29-1996 (ISO4387:1991) standard aspiration filters out, each cambridge filter collects the mainstream smoke total particulate matter of 5 cigarette, formic acid, the Small molecular such as acetic acid and propionic acid low boiling molecule easily passes through cambridge filter, main flume total content is represented by gas gas-phase objects and granule phase substance sum, all the other higher boiling molecules are easily retained by cambridge filter, main flume total content is represented with granule phase substance, take off flue gas supplementary set device, rapidly cambridge filter is taken off, with absorbent cotton wiping supplementary set device, it is together put into triangular flask, add methylene chloride-methanol (volume ratio is 1:4) 50mL, add the mark acetonitrile solution of trans-2-hexenoic acid and each 50 μ L of dichloromethane solution of interior mark hexane diacid in 1.2mg/mL simultaneously, shake up, ultrasonic extraction 15min at 40 DEG C, re-extract is with this, combining extraction liquid, get the organic phase after 1.0mL extraction, with 0.45 μm of filtering with microporous membrane, proceed in 5mL esterification bottle, add the BSTFA of 50 μ L, by organic acid derivatization 50min in 60 DEG C of water-baths, taking-up is cooled to room temperature, proceed to chromatogram bottle analysis.23 kinds of organic acid testing results are respectively in shown in table 1 ~ table 3: what average content propped up more than 100 μ g/ is palmitic acid, formic acid, acetic acid 3 kinds of organic acids, what prop up at 10-100 μ g/ is succinic acid, lactic acid, malic acid and oleic acid 4 kinds of organic acids, what 1-10 μ g/ propped up is 10 kinds of organic acids such as propionic acid, benzoic acid, isovaleric acid, citric acid, oxalic acid, phenylacetic acid, butyric acid, caproic acid, benzenpropanoic acid and isobutyric acid, and 6 kinds of organic acids of remainder are then less than 1 μ g/ and prop up.
Step (2), the identification of the crucial sour odour material of main flume: utilize sense of smell, the sense of taste and Low Flavour Threshold monograph obtain the open report data of these 23 kinds of organic acids in aqueous medium, in the detection data of organic acid content in table 4 associative list 1-table 3, by sense of taste energy value TAV=main flume organic acid content/taste threshold, calculate the sense of taste energy value TAV of each organic acid in 51 increments bases, SPSS software statistics each organic acid TAV >=0.1 sample is adopted to account for the number percent of total sample, the results are shown in Table 5, as shown in Table 5: isovaleric acid, acetic acid, the TAV of valeric acid is greater than 1, formic acid, butyric acid, succinic acid, lactic acid and isobutyric acid are greater than 0.1, and all the other 15 kinds of organic acids are all less than 0.1, from TAV value >=0.1 sample percentage (%), 7 organic acids such as formic acid, acetic acid, butyric acid, isovaleric acid, valeric acid, lactic acid and succinic acid are all 100% in 51 samples, and isobutyric acid is also up to 98.04%.Therefore crucial sour odour material is these 8 kinds of organic acids of formic acid, acetic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid, lactic acid and succinic acid in main flume, concrete sequence is: isovaleric acid > acetic acid > valeric acid > formic acid > butyric acid > succinic acid > isobutyric acid > lactic acid, and other 15 kinds of organic acids such as more than six carbon direct-connected carboxylic acid, aromatic acid and most dibasic acid are almost negligible to the contribution of tart flavour.
Step (3), the foundation of flue gas tart flavour index assessment model: set up the exponential model such as smoke hazard, Maturity of Tobacco Leaf evaluation method based on material base, the quality evaluation of raw tobacco material and cigarette product is made to be that objective quantization signifying becomes possibility from the subjective mode transition of sensory evaluation, the concentrated reflection being tobacco business to quality research and innovation achievement and effective experience.Present patent application uses for reference the experience that index of correlation model is set up, and proposes first and sets up flue gas tart flavour exponential model.From step 2, the crucial sour odour material of main flume is formic acid, acetic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid, lactic acid and succinic acid, by flue gas tart flavour index=each crucial organic acid sense of taste energy value sum, so, flue gas tart flavour index=(isovaleric acid content/0.74+ acetic acid content/50+ valeric acid content/0.50+ formic acid content/160+ butyric acid content/3.19+ succinic acid content/50+ isobutyric acid content/5.0+ lactic acid content/133.2), with the tart flavour index of the method evaluation 51 parts of flue gas samples in " exponential model method " column number in table 6 according to shown in.
Step (4), the evaluation of flue gas tart flavour index assessment model: organize 11-17 name by degree of having a sharp sense of taste test and the technician obtaining cigarette sensory evaluating smoking qualification, human body evaluation is carried out to 51 this flue gas of increment sourness intensity, average and represent the data of sensory evaluation method, in table 6 " sensory evaluation method " column number according to shown in; And adopt Unscrambler 9.7 software to " exponential model method " and " sensory evaluation method " two groups of data dependence inspections, the results are shown in Figure 1.As can be seen from Figure 1, the relative coefficient that exponential model method and sensory evaluation method are evaluated 51 parts of flue gas sample tart flavours is up to 0.919080, show that two kinds of evaluation methods have higher trend consistance, therefore, desirable fitting effect is achieved with human body evaluation assessment, achieve the objective evaluation of flue gas sourness intensity, can be used for the research and development of the announcement of flue gas sense of taste mechanism and cigarette product flavoring technology.
The testing result (μ g/ props up) of this main flume of table 1 51 increment VFA content
The testing result (μ g/ props up) of this main flume of table 2 51 increment half property organic acid content
The testing result (μ g/ props up) of the difficult VFA content of this main flume of table 3 51 increment
Sample number into spectrum Oxalic acid Lactic acid Malic acid Citric acid Succinic acid
1 3.74 38.36 32.19 4.56 56.87
2 3.79 38.81 38.51 4.30 54.14
3 3.60 36.99 30.55 4.71 52.90
4 3.52 36.16 37.32 5.23 47.89
5 3.19 32.82 26.18 6.34 54.53
6 3.63 37.25 35.21 5.57 52.93
7 3.52 36.18 28.07 5.43 53.25
8 3.54 36.39 35.75 4.45 50.94
9 3.39 34.85 35.61 5.51 58.70
10 3.91 40.03 32.41 3.21 49.13
11 3.27 33.65 31.40 4.43 62.41
12 4.16 42.50 26.32 3.33 54.98
13 3.66 37.55 31.14 2.27 53.89
14 3.59 36.83 34.97 6.36 68.34
15 4.55 46.46 39.94 5.72 48.42
16 3.22 33.18 40.41 2.27 59.83
17 3.98 40.78 31.00 5.42 58.27
18 3.88 39.74 21.16 5.39 49.02
19 3.26 33.57 34.24 5.53 66.60
20 4.43 45.29 34.62 3.80 57.77
21 3.18 32.73 34.68 3.55 50.21
22 3.24 33.74 33.24 4.85 47.57
23 2.60 38.92 30.04 4.71 47.89
24 3.49 32.54 29.03 3.73 45.58
25 2.99 41.39 23.95 4.79 53.34
26 2.92 36.44 28.77 2.49 43.77
27 3.88 35.72 32.60 3.71 57.05
28 2.55 45.35 37.57 2.61 49.62
29 3.61 36.11 21.49 6.20 54.16
30 3.66 36.56 31.41 4.29 54.84
31 3.47 34.74 37.73 4.03 52.11
32 3.39 33.91 29.77 4.44 50.87
33 3.06 30.57 36.54 4.96 45.86
34 3.50 35.00 25.40 6.07 52.50
35 3.39 33.93 34.43 5.30 50.90
36 3.41 34.14 27.29 5.16 51.22
37 3.26 32.60 34.97 4.18 48.91
38 3.78 37.78 34.83 5.24 56.67
39 3.14 31.40 31.63 2.94 47.10
40 4.03 40.25 30.62 4.16 60.38
41 3.53 35.30 25.54 3.06 52.95
42 3.46 34.58 30.36 2.00 51.86
43 4.42 44.21 34.19 6.09 66.31
44 3.09 30.93 39.16 5.45 46.39
45 3.85 38.53 39.63 2.00 57.80
46 3.75 37.49 30.22 5.15 56.24
47 3.13 31.32 20.38 5.12 46.99
48 4.30 43.04 33.46 5.26 64.57
49 3.05 30.48 33.84 3.53 45.72
50 3.07 30.75 36.32 1.74 46.12
51 3.74 37.38 39.18 5.65 56.07
The literature values * of table 4 23 kinds of main flume organic acid taste thresholds
Organic acid title Taste threshold (mg/kg) Organic acid title Taste threshold (mg/kg)
Formic acid 160 Myristic acid 5000
Acetic acid 50 Benzoic acid 340
Propionic acid 245 Phenylacetic acid 647
Isobutyric acid 5 Benzenpropanoic acid 755
Butyric acid 3.19 Palmitic acid 5,000
Isovaleric acid 0.74 Oleic acid 1,100
Valeric acid 0.5 Linoleic acid 670
3 methylvaleric acid 30 Leukotrienes 1,000
Caproic acid 81 Oxalic acid 45
Enanthic acid 94 Lactic acid 133.2
Sad 101 Malic acid 87
N-nonanoic acid 10 Citric acid 770
Capric acid 69 Succinic acid 50
Lauric acid 500
*: derive from L.J.van Gemert.Flavour Thresholds, compilatations of flavor threshold values in water and other media (Edition 2011) [M] .Oliemans Punter & Partners BV, Houten, The Netherlands, 2011.
The identification of sense of taste energy value (TAV) statistical study of this main flume of table 5 51 increment organic acid and crucial sour odour material
Table 6 exponential model evaluation assessment and sensory evaluation method are to the evaluation result of 51 this main flume of increment sourness intensity

Claims (6)

1., based on the flue gas tart flavour index assessment method for establishing model of sense of taste energy value, it is characterized in that comprising the steps:
Step (1), the detection of main flume organic acid content: utilize N, two (TMS) trifluoroacetamide derivatization method pretreatment technology of O-and gas chromatograph-mass spectrometer realize the quantitative test of organic acid content in main flume, wherein, Small molecular low boiling molecule easily passes through cambridge filter, represent main flume total content by gas gas-phase objects and granule phase substance sum, all the other higher boiling molecules are easily retained by cambridge filter, represent main flume total content with granule phase substance;
Step (2), the identification of the crucial sour odour material of main flume: the taste threshold that the main flume organic acid content utilizing step (1) to obtain and document are openly reported, calculates each organic acid sense of taste energy value TAV=main flume organic acid content/taste threshold; When certain organic acid TAV >=0.1, then it is identified as the crucial sour odour material in main flume;
Step (3), the foundation of flue gas tart flavour index assessment model: in the main flume obtain step (2), crucial sour odour material TAV sues for peace to set up flue gas tart flavour index assessment model, flue gas tart flavour index=each crucial organic acid sense of taste energy value sum;
Step (4), the evaluation of flue gas tart flavour index assessment model: organize cigarette sense organ technician, human body evaluation is carried out to flue gas sourness intensity, and adopts SPSS or Unscrambler statistical software, score value is evaluated to flue gas tart flavour index and human body and carries out fitting effect analysis.
2. the flue gas tart flavour index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: main flume described in step (1) is the main flume that flammable suction tobacco and tobacco product produce through burning.
3. the flue gas tart flavour index assessment method for establishing model based on sense of taste energy value according to claim 2, is characterized in that: main flume described in step (1) is the main flume that cigarette, cigar, pipe tobacco, redried leaf tobacco, stem or reconstituted tobacoo produce through burning.
4. the flue gas tart flavour index assessment method for establishing model based on sense of taste energy value according to claim 1, it is characterized in that: described in step (1), main flume organic acid comprises three compounds: VFA, partly waving property sends out organic acid and waving property of difficulty sends out organic acid.
5. the flue gas tart flavour index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: the mass analyzer of gas chromatograph-mass spectrometer described in step (1) is any one in commercially available quadrupole rod mass analyzer, ion strap mass analyzer and time of flight mass analyzer.
6. the flue gas tart flavour index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: the experimenter participating in the sensory evaluation of flue gas sourness intensity in step (4) should be the volunteer being tested and obtained cigarette product sensory evaluating smoking technical qualification card by sense of taste susceptibility.
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