coenzyme q10 production by sphingomonas sp

9
J. Microbiol. Biotechnol. (2011), 21(5), 494–502 doi: 10.4014/jmb.1012.12017 First published online 9 April 2011 Coenzyme Q 10 Production by Sphingomonas sp. ZUTE03 with Novel Precursors Isolated from Tobacco Waste in a Two-Phase Conversion System Qiu, Lequan, Weijian Wang, Weihong Zhong * , Li Zhong, Jianjun Fang, Xuanzhen Li, Shijin Wu, and Jianmeng Chen College of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310032, China Received: December 13, 2010 / Revised: January 28, 2011 / Accepted: January 31, 2011 Coenzyme Q 10 (CoQ 10 ) is a widely used supplement in heart diseases treatment or antioxidative dietary. The microbial production of CoQ 10 was enhanced by addition of solanesol and novel precursors recovered from waste tobacco. The novel precursors were separated by silica gel and identified as α-linolenic acid (LNA) and butylated hydroxytoluene (BHT) based on the effect on CoQ 10 production and GC-MS. The effects of novel precursors on CoQ 10 production by Sphingomonas sp. ZUTE03 were further evaluated in a two-phase conversion system. The precursor’s combination of solanesol (70 mg/l) with BHT (30 mg/l) showed the best effect on the improvement of CoQ 10 yield. A maximal CoQ 10 productivity (9.5 mg l -1 h -1 ) was achieved after 8 h conversion, with a molar conversion rate of 92.6% and 92.4% on BHT and solanesol, respectively. The novel precursors, BHT and LNA in crude extracts from waste tobacco leaves, might become potential candidates for application in the industrial production of CoQ 10 by microbes. Keywords: Coenzyme Q 10 , microbial conversion, tobacco waste, precursor, Sphingomonas sp. ZUTE03 Coenzyme Q 10 (CoQ 10 ) has been widely used in treating heart diseases for more than 30 years [12]. Additionally, CoQ 10 shows a variety of physiological activities indicated for hypertension, brain vascular injury, anemia, muscle dystrophy, and alveolar pyorrhea. Recently, CoQ 10 has been used as food supplements owing to its various physiological activities [12, 13]. Extensive attempts have been made to increase the production of CoQ 10 to meet the growing demands of the pharmaceutical industry. CoQ 10 can be produced by chemical synthesis [17], semi-chemical synthesis [15], and microbial fermentation [28]. However, economical production of CoQ 10 by microbes is considered as the most viable approach and has attracted increasing attention of biochemical engineers [3, 4, 11]. The development of strain and the optimization of fermentation strategies and environmental parameters have resulted in yield improvement of CoQ 10 [5-9, 21, 24].There also have been an increasing number of reports on the improvement of CoQ 10 production by molecular biological methods [2, 14, 18, 19, 22, 23, 29-31]. However, the highest yield of CoQ 10 production was achieved by Rhodopseudomonas spheroides with fed-batch process [21], suggesting further studies on metabolic engineering is required to improve CoQ 10 biosynthesis. Meanwhile, both the selection of more effective precursors and the optimization of fermentation/ conversion conditions are still necessary to enhance CoQ 10 production by microbes. It was widely reported that addition of precursors or regulators, such as para-hydroxybenzoic acid (PHB), solanesol, 4-hydroxybenzoic acid, methionine, L-phenylalanine, and tyrosine, could improve the microbial production of CoQ 10 [10, 25]. Some precursors or stimulators are present in the natural plant biomass. For example, carrot juice and tomato juice could be utilized as the natural precursors to enhance the production of CoQ 10 by Pseudomonas diminuta NCIM 2865 [1]. Tobacco biomass hydrolysate could also enhance the CoQ 10 production by Rhodospirillum rubrum [26]. However, tobacco waste was the widely used material to recover solanesol owing to its high content of this traditional precursor for CoQ 10 production [16]. Millions of tons of tobacco waste is produced by the tobacco industry in China per year, which has yet caused environmental problem. Therefore, it is valuable and necessary to study how to recycle such materials. The main strategies to recycle tobacco waste include the reconstitution of tobacco [33], composting the material [20], and the recovery of valuable substances. *Corresponding author Phone: +86-571-88320739; Fax: +86-571-88320739; E-mail: [email protected]

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Page 1: Coenzyme Q10 Production by Sphingomonas Sp

J. Microbiol. Biotechnol. (2011), 21(5), 494–502doi: 10.4014/jmb.1012.12017First published online 9 April 2011

Coenzyme Q10 Production by Sphingomonas sp. ZUTE03 with NovelPrecursors Isolated from Tobacco Waste in a Two-Phase Conversion System

Qiu, Lequan, Weijian Wang, Weihong Zhong*, Li Zhong, Jianjun Fang, Xuanzhen Li, Shijin Wu, andJianmeng Chen

College of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310032, China

Received: December 13, 2010 / Revised: January 28, 2011 / Accepted: January 31, 2011

Coenzyme Q10 (CoQ10) is a widely used supplement in

heart diseases treatment or antioxidative dietary. The

microbial production of CoQ10 was enhanced by addition

of solanesol and novel precursors recovered from waste

tobacco. The novel precursors were separated by silica gel

and identified as α-linolenic acid (LNA) and butylated

hydroxytoluene (BHT) based on the effect on CoQ10

production and GC-MS. The effects of novel precursors

on CoQ10 production by Sphingomonas sp. ZUTE03 were

further evaluated in a two-phase conversion system. The

precursor’s combination of solanesol (70 mg/l) with BHT

(30 mg/l) showed the best effect on the improvement of

CoQ10 yield. A maximal CoQ10 productivity (9.5 mg l-1

h-1

)

was achieved after 8 h conversion, with a molar conversion

rate of 92.6% and 92.4% on BHT and solanesol, respectively.

The novel precursors, BHT and LNA in crude extracts

from waste tobacco leaves, might become potential

candidates for application in the industrial production of

CoQ10 by microbes.

Keywords: Coenzyme Q10, microbial conversion, tobacco

waste, precursor, Sphingomonas sp. ZUTE03

Coenzyme Q10 (CoQ10) has been widely used in treating

heart diseases for more than 30 years [12]. Additionally,

CoQ10 shows a variety of physiological activities indicated

for hypertension, brain vascular injury, anemia, muscle

dystrophy, and alveolar pyorrhea. Recently, CoQ10 has

been used as food supplements owing to its various

physiological activities [12, 13]. Extensive attempts have

been made to increase the production of CoQ10 to meet the

growing demands of the pharmaceutical industry. CoQ10

can be produced by chemical synthesis [17], semi-chemical

synthesis [15], and microbial fermentation [28]. However,

economical production of CoQ10 by microbes is considered

as the most viable approach and has attracted increasing

attention of biochemical engineers [3, 4, 11]. The development

of strain and the optimization of fermentation strategies

and environmental parameters have resulted in yield

improvement of CoQ10 [5-9, 21, 24].There also have been

an increasing number of reports on the improvement of

CoQ10 production by molecular biological methods [2, 14,

18, 19, 22, 23, 29-31]. However, the highest yield of

CoQ10 production was achieved by Rhodopseudomonas

spheroides with fed-batch process [21], suggesting further

studies on metabolic engineering is required to improve

CoQ10 biosynthesis. Meanwhile, both the selection of more

effective precursors and the optimization of fermentation/

conversion conditions are still necessary to enhance CoQ10

production by microbes. It was widely reported that addition

of precursors or regulators, such as para-hydroxybenzoic

acid (PHB), solanesol, 4-hydroxybenzoic acid, methionine,

L-phenylalanine, and tyrosine, could improve the microbial

production of CoQ10 [10, 25].

Some precursors or stimulators are present in the natural

plant biomass. For example, carrot juice and tomato juice

could be utilized as the natural precursors to enhance the

production of CoQ10 by Pseudomonas diminuta NCIM

2865 [1]. Tobacco biomass hydrolysate could also enhance

the CoQ10 production by Rhodospirillum rubrum [26].

However, tobacco waste was the widely used material to

recover solanesol owing to its high content of this traditional

precursor for CoQ10 production [16]. Millions of tons of

tobacco waste is produced by the tobacco industry in China

per year, which has yet caused environmental problem.

Therefore, it is valuable and necessary to study how to

recycle such materials. The main strategies to recycle

tobacco waste include the reconstitution of tobacco [33],

composting the material [20], and the recovery of valuable

substances.

*Corresponding authorPhone: +86-571-88320739; Fax: +86-571-88320739;E-mail: [email protected]

Page 2: Coenzyme Q10 Production by Sphingomonas Sp

495 Qiu et al.

In the present study, we isolated two novel precursors of

CoQ10 from waste tobacco leaves by chance. Their effects

on CoQ10 production were evaluated in a water-organic

solvent, two-phase system, which was designed as the

bioconversion system of CoQ10 directly from precursors

[34]. The bioconversion system might decrease the cost of

downstream purification, because fewer other metabolites

would be extracted into the organic phase. Meanwhile,

such system is also equal to a kind of conversion-extraction

couple process, which might contribute to enhancing the

production of CoQ10. To our knowledge, this is the first

report on CoQ10 production by Sphingomonas sp. ZUTE03,

using novel precursors in a two-phase conversion system.

MATERIALS AND METHODS

Chemicals

Coenzyme Q10 (purity above 99%) was purchased from Wako Pure

Chemical Industries (Osaka, Japan). Solanesol (purity above 95%)

was purchased from Weifang Three Power Group Co. Ltd. (Shandong,

China). Alpha-linolenic acid (purity above 80%) was purchased from

Beijing Health Science and Technology Co. Ltd. (Beijing, China).

Butylated hydroxytoluene (purity above 99.8%) was purchased from

Hangzhou Wanjing Novel Material Co. Ltd. (Hangzhou, China).

Other chemicals were purchased locally.

Strain and Culture Conditions

Sphingomonas sp. ZUTE03, which exhibited excellent coenzyme

Q10 production ability, was isolated from the soil in the banks of

the Qiantang River, Zhejiang Province, China. The strain has been

deposited in the China Center for Type Culture Collection (CCTCC)

at Wuhan University, Wuhan, China, under the accession number

CCTCC M207084.

The seed medium contained 20 g/l glucose, 10 g/l peptone, 10 g/l

yeast extract, and 5 g/l NaCl. The fermentation medium contained

15 g/l glucose, 10 g/l (NH4)2SO4, 1 g/l yeast extract, 0.5 g/l KH2PO4,

1.5 g/l Na2HPO4, 0.5 g/l MgSO4·7H2O. The initial pH of the above

medium was adjusted to 7.0 with 2 M NaOH and the medium was

then autoclaved at 115oC for 30 min.

Culture conditions: One loop of Sphingomonas sp. ZUTE03 from

a slant was inoculated into 100 ml of seed medium in a 250 ml flask

for 24 h incubation at 180 rpm and 28oC. Then, 5 ml of seed

medium was inoculated into 150 ml of fermentation medium in a

500 ml flask. After 12 h cultivation at 180 rpm and 28oC, precursor

samples were added into the broth to afford the final concentration

0.75 g/l and started a consequential 24 h conversion before the final

biomass and CoQ10 yield were measured.

Analytical Method

The extraction of CoQ10 from cells and the biomass measurement

were carried out according to reported methods [32].

The CoQ10 concentration was analyzed by high-performance liquid

chromatography (HPLC) (Type SPD-10AVP; Shimadzu, Japan)

equipped with a ZORBAX SB-C18 column (4.6×250 mm; Agilent,

USA). A mixture of methanol and hexane (83:17 by volume) was

used as the mobile phase at a flow rate of 1.0 ml/min. The UV

detector wavelength was 275 nm and the sampling quantity was 20 µl.

The concentration of solanesol was analyzed by HPLC (Type

SPD-10AVP; Shimadzu, Japan) equipped with a Shim-pack HRC-

SIL column (4.6×150 mm; Shimadzu, Japan). A mixture of hexane

and isopropanol (98:2 by volume) was used as the mobile phase at a

flow rate of 0.5 ml/min. The UV detector wavelength was 215 nm

and the sampling quantity was 20 µl.

The concentration of butylated hydroxytoluene (BHT) was analyzed

by HPLC (Type Agilent 1100, USA) equipped with a ZORBAX SB-

C18 column (4.6×150 mm). Anhydrous ethyl alcohol (chromatographic

grade) was used as the mobile phase at a flow rate of 1.0 ml/min,

The UV detector wavelength was 215 nm and the sampling quantity

was 20 µl.

Extraction of the Crude Solanesol from the Tobacco Waste

Waste tobacco leaves (Hangzhou Liqun Environment Protecting Paper

Co. Ltd., Hangzhou, China) were soaked in the distilled water for

10 h before filtration for removing water-soluble impurities. The wet

material was dried at 100oC for 2 h and then grinded to pieces of

the same size. About 120 g of treated waste tobacco leaves was

immersed in 1,500 ml of petroleum ether and extracted for 10 h at

50oC in a 2 l three-neck bottle with stirring paddle. The organic solvent

was collected by filtration and concentrated by a vacuum rotatory

evaporator to obtain the crude solanesol.

Further Separation of the Crude Solanesol and Effective

Component Analysis

The crude solanesol was saponified by KOH (16 M) at 50oC for 2 h.

After dissolving in petroleum ether, the saponified crude solanesol

was loaded to a silica gel column (4×60 cm, height of silica gel

about 40 cm), and then slowly eluted by petroleum ether. A green-

color substance was first eluted and collected. Then subsequent

colorless substance was eluted with a mixture of petroleum ether

and acetone (9:1 by volume), and collected as 40 ml per tube.

The collected eluent was identified by thin-layer chromatography

(TLC) on silica gel plates (Type GF254; Qingdao Ocean Chemical

Co. Ltd, China) with petroleum ether and ethyl acetate (4:1 by

volume) as the developing solvent and colored by iodine spraying

method. The fraction of eluent with the same Rf value on the silica

gel plates was combined and concentrated. The effects of these

concentrates on CoQ10 fermentation by Sphingomonas sp. ZUTE03

were evaluated. The most effective fractions to improve the CoQ10

production were further separated by silica gel column and analyzed

by TLC, HPLC, and gas chromatography-mass spectrometry (Agilent

5975C GC-MS, USA).

Effects of Possible Novel Precursors on CoQ10 Conversion by

Sphingomonas sp. ZUTE03 in a Two-Phase Conversion System

The results of the previous research [34] showed that coenzyme Q10

production of Sphingomonas sp. ZUTE03 in a water-organic solvent,

two-phase conversion system was superior to the traditional microbial

fermentation. Therefore, the two-phase conversion system was used

in the subsequent study for the effects of possible novel precursors

on CoQ10 conversion by Sphingomonas sp. ZUTE03. The two-phase

conversion system for CoQ10 production was a batch-type cultivation

and designed as follows. One loopful of strain ZUTE03 from a slant

was inoculated into 100 ml of seed medium in a 250 ml flask. After

24 h incubation at 180 rpm and 28oC, cells were harvested by

centrifugation at 4,000 rpm and 4oC for 10 min, and then suspended

in the 25 ml aqueous phase, acetate buffer (0.2 M, pH=4.6), mixed

Page 3: Coenzyme Q10 Production by Sphingomonas Sp

MICOBIAL PRODUCTION OF COQ10 WITH NOVEL PRECURSORS 496

with 25 ml of hexane (as the organic phase) in a 250 ml flask for

the consequential bioconversion at 28oC and 180 rpm. The extract

solvent was collected from the top layer of the broth as the analytical

sample for CoQ10 yield.

Single precursors (100 mg/l, LNA and BHT) and precursor

combination (each 100 mg/l, solanesol and PHB, BHT and solanesol,

LNA and BHT, PHB and LNA) were dissolved in 25 ml of hexane

(as organic phase), respectively. Treatment with no precursors added

served as the control. The solution was then mixed with 25 ml of

acetate buffer (0.2 M, pH 4.6, as water phase) in a 500 ml flask to

form the two-phase conversion system. Then, 170 mg DCW of cells

was inoculated and 1 ml of soybean oil was added as a cell membrane

permeability accelerant. After 8 h conversion at 28oC and 180 rpm,

CoQ10 in the organic solvent was analyzed by HPLC to determine

the most effective treatment with enhanced CoQ10 production.

After the optimal precursor or precursor combination was selected,

the effect of precursor concentration on the CoQ10 production was

evaluated in the two-phase conversion system. To optimize the

precursor concentration and to test the reciprocal effect between the

two different precursors, a double-factor orthogonal experiment using

L9 (3)3 was performed.

Statistical Analysis Methodology

Each treatment in the experiment was performed in triplicate. Software

Origin 8.0 was used to draw the figures with error bars.

RESULTS

Effect of Crude Solanesol on CoQ10 Production by

Sphingomonas sp. ZUTE03

The purity of the crude solanesol, extracted from waste

tobacco leaves was analyzed by HPLC. The results (Fig. 1A

and 1B) showed that the solanesol content in the crude

extracts was 14.43% (by weight). The crude and the standard

solanesols were added to the fermentation medium at the

beginning of cultivation to a final solanesol concentration

of 100 mg/l, respectively. After 36 h culture, biomass and

CoQ10 yield were determined. The results (Fig. 1C) showed

that CoQ10 yield with the addition of crude solanesol

(3.12 mg/l, 1.81 mg/g-DCW) was higher than that with the

addition of standard solanesol (2.03 mg/l, 1.03 mg/g-DCW).

Among all the treatments, the CoQ10 yield of control was

the lowest (1.59 mg/l, 0.98 mg/g-DCW). The results suggested

that something in crude solanesol improved CoQ10 production.

Therefore, crude solanesol was separated with silica gel to

isolate and identify the possible novel active components.

Separation of the Crude Solanesol and Effects of

Eluents on CoQ10 Production

When the crude solanesol was separated with silica gel, one

kind of pigment substance with green color was first eluted

and collected. The subsequent colorless eluents were identified

by TLC with iodine coloring by spraying method. The

results (Fig. 2A) showed that there are no colorable

substances in the eluents of tubes from #1 to #6. The Rf

values of colored substances in tubes #8 to #11 were higher

than that of solanesol, and a small amount of solanesol was

simultaneously eluted. The main colorable substance in

tubes #12 to #20 was solanesol, which gradually decreased

in tubes #21 to #25. The Rf values of the main colorable

substances in tubes #26 to #43 were lower than that of

solanesol. To test the effects of different eluted fractions on

CoQ10 fermentation, the eluents in tubes #21 to #25, the

eluents in tubes #26 to #43, and pigment substance were

combined and concentrated, respectively. Different concentrates

were then added to the fermentation medium after 12 h

culture. Biomass and CoQ10 yield were determined after

36 h of culture and the results are shown in Fig. 2B. The

CoQ10 yield with the concentrate of tubes #26 to #43 as

precursors was the highest (11.73 mg/l, 6.19 mg/g-DCW)

among all the treatments, which was 6.53 times higher

than that of the control, 5.72 times higher than that of

Fig. 1. HPLC analysis of crude extract (A) and solanesol standard(B) and their effects on the CoQ10 yield by Sphingomonas sp.ZUTE03 in fermentation medium (C).

Page 4: Coenzyme Q10 Production by Sphingomonas Sp

497 Qiu et al.

concentrate from tubes #12 to #25, and 1.56 times higher

than that of pigment substance. The above results indicate

that more effective components might be present in the

eluent in tubes #26 to #43 than saolanesol, which was

regarded traditionally as the precursor for CoQ10 production

in tobacco waste.

Further Separation and Analysis of the Effective

Components

To further determine the effective component, the concentrate

from tubes #26 to #43 was further separated on a silica gel

column, identified by TLC, and colored with the iodine

spraying method. The results (Fig. 3A) showed that the

major colorable components were in tubes #12 to #17.

Consequently, the eluents in tubes #12 to #17 were combined,

concentrated, and analyzed by HPLC. The HPLC analysis

(Fig. 3B) showed that there were two main components in

the concentrate, whose retention times were 6.488 min

and 9.715 min, respectively. GC-MS analysis showed that

the concentrate contained two main kinds of substances

(Fig. 3C and 3D), namely LNA, with a structure similar to

solanesol, and BHT, with a benzene ring structure. Based

on their special structure, LNA and BHT would be the

possible precursors of microbial CoQ10 production, which

have never been reported before.

Effects of Novel Precursors on CoQ10 Conversion by

Sphingomonas sp. ZUTE03

Owing to the advantages like less product loss, lower cost

of downstream purification, and higher efficiency [27], over

the traditional microbial fermentation in a complex medium

and chemical synthesis, a two-phase microbial conversion

system was designed to evaluate the effects of novel precursors

on the conversion of CoQ10 by Sphingomonas sp. ZUTE03.

The results of the previous research [34] showed that the

CoQ10 yield with the combination of solanesol and PHB as

precursors was much better than with solanesol or PHB

alone. In this study, the results (Fig. 4) also showed that

CoQ10 yield in precursors combination treatment was

superior to that of precursor alone treatment, and among

all the treatments, the CoQ10 yield of solanesol-BHT

combination treatment was the highest (72.05 mg/l,

Fig. 2. TLC identification of the eluent of crude extract separated by silicon column (A) and the effects of the different eluents on CoQ10

yield by Sphingomonas sp. ZUTE03 in fermentation medium (B) (CK: solanesol standard; 1-43: eluents of tubes #1 to #43).

Page 5: Coenzyme Q10 Production by Sphingomonas Sp

MICOBIAL PRODUCTION OF COQ10 WITH NOVEL PRECURSORS 498

41.81 mg/g-DCW). The novel precursors combination (i.e.,

BHT and LNA) was superior to the traditional precursors

combination) (i.e., solanesol and PHB). Additionally, the

CoQ10 yield of single novel precursor, BHT or LNA, was

at a same level as the combination of solanesol and PHB.

The results also indicated that both BHT and LNA as

precursors were more effective than solanesol or PHB.

However, the combination of solanesol and BHT favored

CoQ10 production the most. Furthermore, BHT, as an

antioxidant capable of preventing the oxidation of CoQ10,

is much cheaper than PHB. Therefore, solanesol and BHT

were selected as the most effective precursors in the further

study.

Effects of Concentrations of BHT and Solanesol on

CoQ10 Conversion

To detect the effects of BHT concentration on CoQ10

production, 20, 30, 40, 50, or 60 mg/l BHT was added

with 100 mg/l solanesol, respectively, at the beginning of

culture for conversion. The results showed that the CoQ10

yield of 30 mg/l BHT treatment was the highest (74.52 mg/l,

Fig. 5A) with the highest conversion ratio of BHT and

solanesol (92.15% and 90.31%, respectively, Fig. 5B),

suggesting that 30 mg/l was the optimal BHT concentration

with a solanesol concentration of 100 mg/l.

Based on the above results, 60, 70, 80, 90, or 100 mg/l

solanesol with 30 mg/l BHT was added respectively at

the beginning of culture to evaluate the effects of BHT

concentration on the CoQ10 conversion. The results showed

that when 70 mg/l solanesol was added, CoQ10 yield was

the highest (75.81 mg/l, Fig. 6A) with the highest conversion

ratio of BHT and solanesol (93.19% and 92.28%, respectively,

Fig. 6B). It suggested that 70 mg/l solanesol with 30 mg/l

BHT might be the optimal concentration for CoQ10 conversion

by Sphingomonas sp. ZUTE03 in the two-phase conversion

system.

Fig. 3. Further separation by silicon column and identification ofthe eluent with lower Rf than solanesol (in tubes #26 to #43 inFig. 2A) by TLC (A), HPLC (B), and GC-MS (C, D) (CK:solanesol standard; 1-24: further separated eluent tubes).

Fig. 4. Effects of precursors on the CoQ10 production bySphingomonas sp. ZUTE03 in a two-phase conversion system.

Page 6: Coenzyme Q10 Production by Sphingomonas Sp

499 Qiu et al.

In addition to CoQ10 yield and molar conversion rate,

the residual precursor should be taken into consideration

simultaneously to evaluate the process condition of CoQ10

conversion from precursors. Therefore, the optimization of

precursor concentration for CoQ10 production was conducted

based on CoQ10 yield, molar conversion rate of precursor,

and the residual precursor, simultaneously. Meanwhile, the

reciprocal effect between solanesol and BHT should also

be evaluated. In the present study, a double-factor orthogonal

experiment using L9 (3)3 was designed to optimize precursor

concentration and evaluate the effect of the reciprocal

effect between solanesol and BHT on the CoQ10 yield. The

results (Table 1) indicated that both solanesol and BHT

had stronger effects on the CoQ10 yield (larger margin,

RA, B, C of solanesol = 5.5, 2.1, 2.7; RA, B, C of BHT = 3.1, 2.7,

3.1) than the reciprocal effect between solanesol and BHT

(smaller margin, RA, B, C = 1.8, 0.5, 0.6). Thus, the optimal

additional concentrations could be determined by the k

values of solanesol and BHT, which were 70 and 30 mg/l,

respectively (Table 1). Under the optimal concentration,

the maximal CoQ10 yield reached 76.1 mg/l after 8 h

conversion, with a molar conversion rate of 92.6% (on

BHT) and 92.4% (on solanesol), respectively. It was also

concluded that the maximal volumetric productivity of

Sphingomonas sp. ZUTE03 in the two-phase conversion

system could reach 9.5 mg l-1 h-1.

DISCUSSION

The exciting finding in the present study was that two novel

precursors, identified as LNA and BHT, were isolated from

tobacco waste. Both LNA and BHT were more effective

than solanesol in improvement of the CoQ10 yield by

Sphingomonas sp. ZUTE03. Moreover, the addition of

precursors combinations showed more positive effect on

Fig. 5. Effects of BHT concentration on the CoQ10 yield (A) andmolar conversion rate of CoQ10 (B) by Sphingomonas sp.ZUTE03 in a two-phase conversion system.

Fig. 6. Effects of solanesol concentration on the CoQ10 yield (A)and molar conversion rate of CoQ10 (B) by Sphingomonas sp.ZUTE03 in a two-phase conversion system.

Page 7: Coenzyme Q10 Production by Sphingomonas Sp

COENZYME Q

10 P

RODUCTIO

N BY

SPHINGOMONAS S

P. ZU

TE

03 W

ITH

NOVEL P

RECURSORS I

SOLATED

FROM

TOBACCO

WASTE

500

Table 1. Orthogonal test design by L9(3)3 and results.

Sample Solanesol, mg/l (level) BHT, mg/l (level) Solanesol/BHTa (level)CoQ10 yield,

(A) mg/l

Molar conversion

rateb,

CoQ10/BHT, (B) %

Molar conversion

rate,CoQ10/Sol

(C) %

ResidueBHT, (D)mg/l

Residue solanesol,(E) mg/l

1

2

3

4

5

6

7

8

9

65(1)

65(1)

65(1)

70(2)

70(2)

70(2)

75(3)

75(3)

75(3)

25(1)

30(2)

35(3)

25(1)

30(2)

35(3)

25(1)

30(2)

35(3)

(1)

(2)

(3)

(2)

(3)

(1)

(3)

(1)

(2)

66.8

69.6

69.1

70.4

76.1

74.9

73.9

74.6

73.6

87.9

89.8

89.6

89.2

92.6

91.8

88.8

91.5

90.8

86.8

88.9

88.6

88.4

92.4

91.5

87.8

91.2

90.4

5.4

10.2

15.4

5.9

9.2

14.3

3.6

9.2

14.4

9.0

7.9

7.9

11.6

9.7

10.2

13.8

15.2

15.4

A B C D E A B C D E A B C D E

K1

K2

K3

k1

k2

k3

R

205.5

221.4

222.1

68.5

73.8

74.0

5.5

267.3

273.6

271.1

89.1

91.2

90.4

2.1

264.3

272.3

269.4

88.1

90.8

89.8

2.7

31.0

29.6

27.2

10.3

9.9

9.1

1.2

24.8

31.5

44.4

8.3

10.5

14.8

6.5

211.1

220.6

217.6

70.4

73.5

72.5

3.1

265.9

273.9

272.2

88.6

91.3

90.7

2.7

263.0

272.5

270.5

87.7

90.8

90.2

3.1

14.9

28.6

44.1

5.0

9.5

14.7

9.7

34.4

32.8

33.5

11.5

10.9

11.2

0.6

216.3

213.6

219.1

72.1

71.2

73.0

1.8

271.2

269.8

271.0

90.4

89.9

90.3

0.5

269.5

267.7

268.8

89.8

89.2

89.6

0.6

28.9

30.5

28.2

9.6

10.2

9.4

0.8

34.4

34.9

31.4

11.5

11.6

10.5

1.1

aReciprocal effect between solanesol and BHT.bMolar conversion rate: CoQ10 quantity (calculated as molar number) / reduced quantity of precursor (calculated as molar number).

K, Sum A, B, C, D, E of different factors at the same level.

k, The average of K.

R, The difference between the maximum and minimum k values.

Page 8: Coenzyme Q10 Production by Sphingomonas Sp

501 Qiu et al.

CoQ10 production than single precursor, and the combinational

addition of solanesol and BHT improved the CoQ10 yield

most significantly.

Based on the special structure of LNA and BHT (i.e., a

structure similar to solanesol, and a benzene ring structure

similar to PHB), LNA and BHT would be the potential

precursors of microbial CoQ10 production, which have

never been reported before. Usually, it could be proved by

radioactive labeling experimental data that they are exactly

the precursor. However, in the two-phase system, BHT and

LNA were the only chemicals with benzene-ring and the

side chain similar to the structure of CoQ10, respectively.

Thus, the most possible usage of BHT or LNA is as a

precursor of CoQ10. Specifically, we found that the maximal

CoQ10 yield reached 76.1 mg/l after 8 h conversion, with a

nearly equal molar conversion rate of 92.6% (on BHT) and

92.4% (on solanesol), respectively. It suggested that they

possibly incorporated in the CoQ10 structure with a

proportion of 1:1. However, not all the used compounds

were incorporated into CoQ10, some of which (about 8%)

might be utilized as substrates for cell basic metabolism or

other necessary reaction to support the conversion of BHT

and solanesol to CoQ10.

So far, several precursors such as solanesol, PHB,

methionine, L-phenylalanine, and tyrosine have been used

in CoQ10 synthesis. However, most attention was paid on

solanesol and PHB, because the chemical structure of

solanesol was similar to the CoQ10 side chain (isoprene

pyrophosphate), and PHB could be used as a precursor of

the quinone ring of CoQ10. Solanesol is usually regarded as

the main precursor recovered from waste tobacco leaves

owing to its high content in tobacco leaves [16]. However,

we found that there were at least another two novel

precursors in crude extracts from waste tobacco leaves,

namely BHT and LNA, which might provide the benzene

ring structure and side chain similar to the solanesol,

respectively, for CoQ10 synthesis.

The CoQ10 yield in the present study seemed to be

higher than that in previous report about precursor effect

on CoQ10 production, probably either due to the high

efficiency of novel precursors or the two-phase process [1,

16, 26]. Moreover, the maximal volumetric productivity of

Sphingomonas sp. ZUTE03 in the two-phase conversion

system (9.5 mg l-1 h-1) was higher than that of R. spheroides

with fed-batch process (5.1 mg l-1 h-1), although the latter

showed the highest CoQ10 yield (770 mg/l) among all the

previous literature [4, 21]. Therefore, the novel precursors,

BHT and LNA in crude extracts from waste tobacco leaves,

might become the potential candidates for application in

industrial production of CoQ10 by microbes.

However, it is still necessary to increase the CoQ10 yield

and decrease the residual precursor concentration. We

will design a repeat or continuous bioreactor for CoQ10

bioconversion in a two-phase system in our future study,

aimed at recycling of residual precursors. In addition, the

process optimization of economical preparation of novel

precursors from waste tobacco is also necessary and would

be favorable to its potential application in the more economical

microbial production of CoQ10.

Acknowledgment

This study was supported by the Science and Technology

Department of Zhejiang Province of P.R. China under Grant

No. 2007C23035, for which the authors are grateful.

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