[Pollinator] Cell death localization in situ in laboratory reared honey bee (Apis mellifera L

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Tue Feb 1 15:05:04 PST 2011


Paper attached and embedded  below.  Important new information.  Laurie



 
  
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 From: Gerald.Hayes at freshfromflorida.com
To: Ladadams at aol.com
Sent:  2/1/2011 10:21:06 A.M. Pacific Standard Time
Subj: Paper



Take a look at the attached when you get a chance.   Thanks  Jerry 
G. W. Hayes,  Jr. 
Chief, 
Apiary Inspection  Section 
Division of Plant  Industry 
P O Bx  147100 
Gainesville   FL  32614-7100 
(352) 372-3505 ext  128 
email:gerald.hayes at freshfromflorida.com 
Please note that  Florida has a broad public records law (Chapter 119, 
Florida Statutes). Most  written communications to or from state employees are 
public records  obtainable by the public upon request. emails sent to me at 
this email address  may be considered public and will only be withheld from 
disclosure if deeemed  confidential pursuant to the laws of the State of  
Florida. 
Cell  death localization in situ in  laboratory reared honey bee (Apis  
mellifera L.) larvae treated with pesticides 
Ales  Gregorc*,  James D. Ellis 
Honey  Bee Research and Extension Laboratory, Department of Entomology and  
Nematology, University of Florida, P.O. Box 110620, Bldg 970 Natural Area  
Drive, Gainesville, FL, USA 32611 
*Corresponding  author email and present mail address: 
_ales.gregorc at kis.si_ (mailto:ales.gregorc at kis.si) ; Agricultural Institute of  Slovenia, 
Hacquetova 17, SI-1000  Ljubljana, Slovenia, tel:  +386-1- 28 05  150   

Abstract 
In  this study, cell death detected by DNA fragmentation labeling and  
phosphatidylserine (PS) localization was investigated in the honey bee (Apis 
mellifera L.) midgut, salivary  glands and ovaries after treating larvae with 
different pesticides offered via  an artificial diet. To do this, honey bee 
larvae reared in an incubator were  exposed to one of nine pesticides: 
chlorpyrifos, imidacloprid, amitraz,  fluvalinate, coumaphos, myclobutanil, 
chlorothalonil, glyphosate and simazine.  Following this, larvae were fixed and 
prepared for immunohistologically  detected cellular death using two TUNEL 
techniques for DNA fragmentation  labeling and Annexin V to detect the 
localization of  exposed PS specific in situ binding to apoptotic cells.  Untreated 
larvae experienced ~10% midgut apoptotic cell death under controlled  
conditions. All applied pesticides triggered an increase in apoptosis in  treated 
compared to untreated larvae. The level of cell death in the midgut of  
simazine-treated larvae was highest at 77% mortality and statistically similar  
to the level of cell death for chlorpyrifos (65%), imidacloprid (61%),  
myclobutanil (69%), and glyphosate (69%) treated larvae. Larvae exposed to  
fluvalinate had the lowest midgut columnar apoptotic cell death (30%) of any  
pesticide treated larvae. Indications of elevated apoptotic cell death in  
salivary glands and ovaries after pesticides applications were detected.  
Annexin V localization, indicative of apoptotic cell deletion, had an  extensive 
distribution in the midgut, salivary glands and ovaries of  
pesticide-treated larvae. The data suggest that the tested pesticides induced  apoptosis in 
tissues of honey bee larvae at the tested concentrations. Cell  death 
localization as a tool for a monitoring the subclinical and sub-lethal  effects of 
external influences on honey bee larval tissues is discussed.   
Keywords: Apis mellifera, immunohistology, cell  death, TUNEL, insecticide, 
herbicide, fungicide 
Introduction 
Globally,  the environment around honey bee (Apis  mellifera) colonies can 
be contaminated with toxic chemicals from  industrial, agricultural and 
domestic activities. In many cases, these  chemicals are pesticides which 
encompass an array of compounds designed to  repel or kill insects (insecticides), 
plants (herbicides), fungi (fungicides)  and other organisms considered 
pests. Though honey bees are non-target  organisms for most pesticide 
applications, they nevertheless can be exposed to  pesticides while collecting pollen 
and nectar from flowers, collecting resins  from various plants, drinking 
water from rivers/lakes/ponds/etc., breathing,  and during flight (if the 
pesticides are airborne). These pesticides may be  brought back inadvertently 
to the colony where their levels are concentrated  further in the waxy nest 
infrastructure. In surveys of North American honey  bee colonies conducted in 
2007 and 2008, investigators found 121 different  pesticides and 
metabolites in wax, pollen, bees, and corresponding hive  samples [1],  thus 
illustrating the need to understand how pesticides may affect individual  honey bees 
and the social colonies in which they  reside. 
Many  of the pesticides to which honey bees are exposed have insecticidal 
properties  and may be harmful to bees. For example, pesticides are known to 
lower the  developmental rate of queen honey bees, increase the occurrence 
of queen  rejection, and lower queen weight [2-4],  affect honey bee 
cardiotoxicity [5],  and affect forager bee mobility and communicative capacity [6], 
 all among other effects documented in the literature. In our effort, we  
broaden the study of pesticide effects on honey bees by investigating  
pesticide effects on cell death and localization in pesticide-treated, honey  bee 
larvae. 
There  are many reasons to look at pesticide effects in bee larvae tissues. 
First,  toxic effects of pesticides have been shown to manifest in 
mammalian tissue  and alter enzymatic levels, blood biochemistry and tissue 
histology  [7],  thus providing evidence that toxins can affect tissues in 
pesticide-exposed  organisms. Second, histological  changes in treated individuals 
provide a rapid detection method for the  effects of toxicants, especially 
chronic irritants, in various tissues and  organs [8].  Third, many of the 
studies where the effects of pesticides on honey bees are  discussed focus on 
toxin effects on adult bees rather than immature ones,  resulting in a lack of 
information concerning the latter. Fourth, previous  immunocytochemical 
studies of cell death and the localization of heat-shock  proteins in larval 
honey bee tissues after acaricide application have fostered  a 
better-understanding the adverse effects acaricides may have on bees  [9-11].  Finally, 
there is an overall lack of histopathological studies on pesticide  treated 
animal tissues. For all of these reasons, we studied the effects of  pesticides 
on larval honey bees at the cellular level.   
To  determine pesticide effects on the cellular tissues of larval honey 
bees, we  looked specifically at unintentional cell death (necrosis) and 
programmed cell  death (apoptosis) 
[12].  Necrotic cell death is induced by external influences with evident  
morphological changes: i.e. the chromatin condenses and clumps are formed at 
 the nuclear periphery [12].  Necrosis refers to the post mortem changes 
that occur following the  death of the cell [13].  Apoptosis on the other hand 
presents a range of morphological symptoms  including cell shrinkage and 
chromatin margination, the latter of which is  followed by DNA fragmentation 
and the formation of apoptotic bodies  [14].  Apoptosis originally was 
defined as the physiological death of cells and  tissues associated with 
developmental remodeling [15]  and can be induced by genetic [16] and  non-genetic 
[17]  means.   
We  used multiple cell death assays to determine the effects of various 
pesticides  on honey bee larvae. The first method we used to determine the 
progression of  cell death in situ was the TUNEL  (terminal deoxynucleotidyl 
transferase–mediated dUTP nick end-labeling) method  which assesses DNA 
breakdown preceding the nuclear collapse of apoptotic  nuclei [18]  and  consists 
of the visualization of fragmented DNA in the nucleus [19].  Cell death 
previously has been characterized using the terminal TUNEL  technique method in 
the honey bee midgut [10, 20] and  larval salivary glands [11]  where the 
death of salivary gland tissues in honey bee larvae was detected  [21]. We 
decided to use two TUNEL methods in our experiment because others  have provided 
data which show that different TUNEL kits can indicate different  levels of 
cell death in target tissues [10].  For example, the in situ cell death  
detection kit AP was unable to differentiate between apoptosis and necrosis in 
 different human tissues and detected both [22].  Furthermore, DNA 
fragmentation and a TUNEL-positive reaction can occur after  different kinds of cell 
death using various kits. Regardless, immunocytochemical  methods assaying 
DNA fragmentation [24] are useful techniques for detecting  impending 
apoptosis due to larval exposure to pesticides while feeding  [25].   
The  second method we employed to monitor cell death was via our use of 
Annexin V  to detect the localization of exposed phosphatidylserine (PS) 
specific in  vivo binding to apoptotic cells. In dying cells, PS is externalized  
actively to the plasma membrane’s outer leaflet parallel to the 
extracellular  environment [26].  Most forms of cell death share the phenomenon of cell 
surface expression of PS  [27].  Externalization of PS is an early event in 
the sequence of steps leading to  cell death which starts well before 
changes in the cell nuclei and plasma  membrane integrity are compromised [28].  
PS on the cell surface can be detected using Annexin V, a member of the  
annexin protein family that binds in a calcium-dependent way to PS-containing  
membranes [29].  The Annexin V affinity assay discriminates among living 
cells, cells in the  early phase of cell death and (secondary) necrotic cells 
that have a  compromised cell membrane [30].   
In  our study, induced cell death and PS localization was investigated in 
honey  bee midguts after treating larvae with one of nine different 
pesticides  offered via an artificial diet. The tested pesticides (with insecticide 
class  in parentheses) included 2 fungicides [myclobutanil (azole), 
chlorothalonil  (substituted benzene)], 2 herbicides [simazine (triazine), glyphosate 
 (phosphonoglycine)], and 5 insecticides/miticides [fluvalinate 
(pyrethroid),  imidacloprid (nicotinoid), coumaphos (organophosphate), chlorpyrifos  
(organophosphate), amitraz (amidine)] and represent a range of  
modes-of-actions and pesticide families. With the exception of glyphosate, all  have been 
found as residues in honey bee colonies [1].  Immunohistological methods 
using both TUNEL assays and Annexin 5 were employed  in order to reduce the 
probability of extraneous artifacts [25],  in an attempt to define the specific 
modes of cell death, and for the broad  quantification of cell death 
observed in larval midguts. We hypothesized that  increased apoptotic cell death 
(determined using the TUNEL technique) occurs  in pesticide treated larvae in 
comparison to untreated larvae and that PS  exposure on the plasma membrane 
of apoptotic cells (determined using Annexin  V) would be present in 
pesticide treated larvae. 
2.  Materials and Methods 
2.1. Larval rearing, treatment and  sampling 
Experiments were conducted at the University of Florida Honey Bee  Research 
and Extension Laboratory, Department of Entomology and Nematology,  
Gainesville, FL. Queens in three production honey bee colonies housed in  10-frame 
Langstroth-style equipment were confined to a section of newly-drawn  comb 
using a metal queen excluder cage (~10 × 10 × 3 cm) at time t = -12 h. The  
caged queen and frame were returned to the center of the brood nest where  
worker bees could access and tend the queen. After 24 h of queen confinement,  
t = 12 h [ 31,  32], we removed the queen from the cage and replaced the  
cage on the comb as before but this time for 108 h (from t = 0) to allow the  
eggs to hatch and larvae to reach an appropriate age for grafting. During 
this  time, worker bees were able to access the comb to feed the developing 
larvae.  At 108 h, we removed the test frames (now containing 36 ± 12 h old 
larvae) from the colonies and took them to  the laboratory.  
At  the laboratory, the larvae were grafted to sterile, 96-well tissue 
culture  plates (well volume = 0.32 mL, Fisher Scientific, Pittsburgh, PA, USA). 
Prior to grafting the larvae  into plates, we pipetted 20 µL of larval diet 
into the bottom of each cell.  The diet had a pH that ranged from 4.0-4.5 
and consisted of 50% royal jelly  (Glory Bee Foods, Eugene, OR, USA), 6% 
D-glucose (Fischer Chemical, Fair Lawn, NJ,  USA), 6% D-fructose  (Fischer 
Chemical, Fair Lawn, NJ), 37% double distilled water, and 1% yeast extract  (Bacto
™, Sparks,  MD, USA) by volume [32].  Prior to adding the diet to each 
cell, we pre-warmed it to 35oC in  an incubator (Percival Scientific Inc, Perry, 
IA,  USA). 
Each  subsequent day, we transferred larvae to a clean culture plate 
provisioned  with fresh diet. The amount of artificial diet provided to each larva 
depended  on the larva’s age. We fed larvae 20 µL of diet at hours 108 and 
132, 30 µL on  hour 156, 40 µL on hour 180, and 50 µL on hour 204 [33, 34].  
At 204 h post oviposition (larvae are 132 ± 12  h old), we transferred the 
larvae to a 48-well plate (Becton Dickinson  Labware, Franklin Lakes, NJ, 
USA, wells were 13 ×  17 mm)  because the growing larvae were too large to 
handle delicately in a 96-well  plate. Throughout the study, trays containing 
larvae were incubated in the  dark at 35oC and ~96% RH [31].   
To  test the effects of pesticides on developing larvae, specific pesticide 
 concentrations were mixed with the larval diet daily for 4 days beginning 
the  second day larvae were in the laboratory (132 h = 60 h old larvae). 
Nine  treatment groups of larvae were established in all, each group being 
composed  of 12 treated larvae. Each group of test larvae was treated with 1 of 
the  following pesticide doses: 1.6 ppm chlorpyrifos, 400 ppm imidacloprid, 
400 ppm  amitraz, 200 ppm fluvalinate, 100 ppm coumaphos, 400 ppm 
myclobutanil, 400 ppm  chlorothalonil, 400 ppm glyphosate, and 400 ppm simazine. The 
respective  pesticide doses are at or below LC50 values known for honey bee  
larvae (unpublished data). Originally, we wanted to standardize the dose  
delivered across all pesticides at 400 ppm to bracket the upper residue limit  
that any of these pesticides have been found in honey bee colonies [1].  
However, chlorpyrifos has a low LC50 value and  fluvalinate/coumaphos LC50 
values do not fit standard toxicity  curves (unpublished data). As such, these 
three pesticides were administered  at different doses than were the other 
pesticides. All applied pesticides were  obtained from Chem Service, West  
Chester, PA, USA.  
Prior  to administration to the larval diet, each pesticide was diluted 
individually  in an acetone solvent. The diet/pesticide combinations were 
prepared and  stored in 1.5 ml snap-top plastic vials (Fisher Scientific, 
Pittsburgh, PA, USA). We included two control  groups in the study: larvae feeding 
on diet containing acetone and larvae  feeding on an untreated diet. All 
larvae were sampled on day 6 (h = 228), 24  hours after the application of the 
last pesticide treatment. Sampled larvae  were fixed in 10% formalin for 24 
h, dehydrated in a series of alcohols and  xylene, and finally embedded in 
paraffin wax as described by Gregorc and Bowen  [9].  Sections of 5 μm were 
cut on a 2030 Rechert/Young Microtome (Cambridge  Instrument GmbH., Germany), 
 floated on distilled water at 40°C, collected on cleaned slides, and  kept 
in an drying oven at 60°C for ~4 h. Slides then were stored  at room 
temperature until later analyses. 
2.2.  Immunohistology 
The  paraffin wax was removed from the tissue sections in three washes of 
xylene  and three washes of absolute alcohol. Sections then were rinsed in 
Phosphate  Buffer Solution (PBS,  0.01  M, pH 7.1) and  prepared for staining. 
2.3.  DeadEnd colorimetric TUNEL system 
The DeadEnd system (Promega, Madison, WI,  USA) labels  fragmented DNA of 
apoptotic cells in  situ using the TUNEL assay. After applying proteinase K, 
the larval  sections were incubated with the TdT reaction mixture and then 
with a  horseradish peroxidase-labeled streptavidin solution. 
Diaminobenzidine (DAB)  substrate was applied onto the tissue sections to develop a brown 
reaction  product. The sections were counterstained with Mayer’s  
hematoxylin.  Negative control labeling was achieved by substituting the 
deoxynucleotidyl  transferase (TdT) enzyme with PBS. 
2.4.  In  situ cell death detection kit, AP  (ISCDDK) 
Dewaxed  and rehydrated tissue sections were incubated with proteinase K 
(20 μg/mL in  10 mM  Tris/HCl, pH 7.4). Labeling was conducted by covering the 
tissue section with  a TUNEL reaction mixture composed of terminal 
deoxynucleotidyl transferase  (TdT) from calf thymus. TdT enzymes with fluorescein 
were detected using  “converter-AP” consisting of anti-fluorescein 
antibodies from sheep,  conjugated with alkaline phosphatase. The substrate solution 
was obtained  using a Vector® Red Alkaline Phosphatase Substrate Kit (Vector 
Laboratories,  Burlingame, CA, USA). Sections were incubated with  the 
substrate (AP) and washed in tap water for 5 min. Counterstaining was  
accomplished by transferring the sections into Mayer’s hematoxylin and then  rinsing 
the sections under running tap water. As a negative control, we  labeled a 
subgroup with terminal transferase, rather than TUNEL reaction  mixture. 
2.5.  Quantification of cell type and apoptosis 
TUNEL  labeled tissue slides were used for quantification of cell type and 
apoptosis  as determined using Dead End and ISDDK kits. For each treated 
group of larvae,  approximately 300 total cells from at least three larvae on 
different slides  were counted in random fields within the tissue. The 
results were expressed as  the proportion of cells counted that gave positive 
staining. To confirm  reproducibility, 25% of the slides were chosen randomly 
and scored twice. The  proportion of cells that gave positive staining was 
analyzed by treatment (9  pesticides and 2 controls) with a one way ANOVA for 
both staining techniques  (Dead End and ISDDK). Furthermore, we used a two 
way ANOVA to test the effects  of technique, overall treatment and the 
interaction of treatment × technique  on the proportion of cells with positive 
staining. Prior to all analyses, the  proportion data were transformed with an 
asin √x transformation. The  untransformed means are reported in the 
manuscript. Where necessary, we used  Student’s T-tests to compare means, accepting 
differences at P ≤  0.05. 
2.6.  Immunohistochemical localization of  PS 
Dewaxed  and rehydrated tissue sections were placed in PBS (0.01 M, pH 7.1) 
and  incubated with a primary antibody solution. Rabbit antibodies 
polyclonal to  Annexin V were obtained from Abcam  (Abcam Inc., Cambridge,  MA, 
USA). Antibodies were used at a  concentration of 2 µg/ml in PBS with 1% bovine 
serum albumin. After incubating the primary  antibodies overnight at  4°C, 
the  sections were covered with biotinylated universal secondary antibodies 
for 30  min. Alkaline phosphatase reagent also was applied for 30 min. Both 
reagents  were obtained in the Vecastain Universal ABC-AP kit (Vector 
Laboratories,  Burlingame, CA, USA). The substrate solution was  obtained using the 
Vector® Red Alkaline Phosphatase Substrate Kit (Vector  Laboratories, 
Burlingame,  CA, USA). Sections were incubated with  the substrate (AP) and 
counterstaining was accomplished by transferring  sections into Mayer’s 
hematoxylin. As a control, no  primary antibody was applied to the tissue sections. 
Sections  were mounted in Faramount aqueous mounting medium (Dako, 
Carpinteria,  CA, USA).  All slides were examined with a Leica light microscope (Leica 
 Microsystems, Germany)  at 400× magnification. 
3.      Results 
3.1.  DeadEnd colorimetric TUNEL system 
The  brown reaction product obtained from the Promega DeadEnd kit indicated 
 DAB-positive, impending apoptotic cell death in all test larvae. Pesticide 
 specific levels of apoptosis detected in the midgut tissue are shown in 
Table  1. The DAB reaction product was detected in the midguts of all  
pesticide-treated larvae in larger percentages than in control larvae fed  either a 
diet containing acetone or pure diet (Table 1). In all DAB-positive  cells, 
the brown reaction product was localized to the nuclei. The largest  
percentages of DAB-positive cells in the midgut epithelium were observed in  
larvae exposed to simazine, glyphosate, myclobutanil and amitraz (>60%,  Table 
1). There were some incongruities between the two TUNEL techniques used  to 
estimate cell mortality, but these usually were orders of magnitude  
differences in the data because the trends detected by both TUNEL techniques  were 
similar (Table 1). In general, pesticides that resulted in high levels of  
apoptosis as detected by the ISDDK technique resulted in the same as detected  
by the DeadEnd technique (Table 1). Notably, fluvalinate, on average, 
resulted  in the lowest level of apoptosis of any tested pesticide (Table 1).   
The  DAB reaction product was observed in columnar midgut epithelial cells 
in  simazine treated larvae (Fig. 1A) and in nearly all of the regenerative 
cells  in chlorpyrifos treated larvae (Fig. 1B). Furthermore, there were 
midgut  regions in amitraz treated larvae with both DAB-positive columnar and  
regenerative epithelial cells (Fig. 1C), and regions in imidacloprid treated 
 larvae with columnar DAB-positive and regenerative negative cells (Fig. 
1D).  In larvae with high proportions of DAB-positive cells, the positive 
cells were  localized in compartmental areas of the midgut, but tissues also 
were observed  containing only solitary DAB-positive cells (chlorothalonil 
treated larvae,  Fig. 1E). In untreated larvae, ~10% of the midgut epithelial 
cells were  DAB-positive (Fig. 1F).  
The  DAB reaction product also was localized in the salivary glands and the 
ovaries  of treated larvae. Salivary gland tissue expressed high levels of 
DAB-positive  cells in larvae exposed to amitraz (Fig. 1G). Similar levels 
also were found  in salivary glands in simazine, imidacloprid, glyphosate, 
myclobutanil or  fluvalinate treated larvae. In the ovarian tissue, high 
levels of DAB-positive  nurse cells were found in imidacloprid-treated larvae 
(Fig. 1H). In ovaries of  larvae treated with the remaining pesticides, the DAB 
reaction product was  found in similar amounts as in ovaries of untreated 
larvae. At normal tissue  turnover, up to 20% of nurse cells were 
DAB-positive (Fig. 1I). Negative  control sections showed no presence of the DAB 
reaction product, and  endogenous peroxidase also was quenched successfully (Fig. 
1J).   
3.2.  In  situ cell death detection kit, AP  (ISCDDK) 
Twenty-four  hours after honey bee larvae were exposed to the last of four 
pesticide  treatments, the red azo-dye reaction product was found in 
increased levels of  the midgut columnar-cell nuclei and also in the midgut 
regenerative-epithelial  cells. In chlorpyrifos-treated larvae, the level of 
positive-reaction product  in the columnar midgut cells (Fig. 2A) had risen to 
~74% (Table 1). In  simazine, myclobutanil, imidacloprid, chlorpyrifos, 
chlorothalonil and  glyphosate-treated larvae, the level of positive columnar 
epithelial cells  with red azo-dye reaction product was ≥65% (Table 1). Simazine 
induced  localization of red azo-dye reaction product to the columnar and 
regenerative  cells (Fig. 2B). In coumaphos-treated larvae, the reaction 
product was found  in ~48% of all columnar and regenerative epithelial cells 
(Fig.  2C). The  reaction product in the salivary glands was found in 
myclobutanil-treated  larvae, where a majority of cells were positive (Fig. 2D). In 
untreated  larvae, low amounts of reaction products were observed, though 
sporadic cells  were positive (Fig. 2E). The red azo-dye product in the ovarian 
tissue of all  treated and untreated control larvae ranged from 5 to 10 % 
(Fig.  2F).    
3.3.  Immunohistochemical localization of PS 
In  the pesticide-treated larvae, the red azo-dye reaction product detected 
by  Annexin V, which characteristically localizes PS, was found to be 
present  abundantly in the midgut epithelium, salivary glands and ovaries. Thus, 
it was  possible to delineate the PS boundary at the apical columnar cell 
membrane in  the brush border and at the basal cell cytoplasm bound to basal 
membrane by  immunostaining of Annexin V. The Red azo-dye reaction product 
was localized  and bound to the apical brush border in chlorpyrifos- treated 
larvae (Fig.  3A). Annexin V staining spread throughout the midgut epithelium 
cells  noticeably, where immunostaining was diffuse and the entire cell 
cytoplasm of  glyphosate-treated tissue was stained (Fig. 3B). In the 
glyphosate-treated  larvae, Annexin V was abundant and PS was localized in the basal 
and apical  cell cytoplasm (Fig. 3C). Staining of the cytoplasm in a group  
of columnar cells at the basal area was uneven and spotty and bound to the  
basal membrane in simazine-treated larvae (Fig. 3D). Red azo-dye was present 
 abundantly in salivary glands of mycobutanil (Fig. 3E) and ovaries of  
glyphosate-treated larvae (Fig. 3F). Staining was less intensive in  salivary 
gland cells in untreated larvae (Fig. 3G). In untreated larvae,  Annexin V 
was present in some sections of the midgut epithelium and  immunostainning was 
bound to the apical and basal cell membrane (Fig. 3H)  while the cytoplasm 
of the midgut cells was not stained. Results indicate that  Annexin V binds 
to cells of the midgut, salivary glands and ovaries of all  pesticide 
treated larvae abundantly while in untreated larvae Annexin V  binding was not as 
evident. In both groups of control larvae, the general  morphology of the 
epithelium was unchanged. 
4.      Discussion 
Honey  bee larvae reared in an incubator and treated with one of nine 
pesticides  undergo subclinical, cellular changes that can be detected using  
immunohistochemical methods. ISCDDK showed comparable levels of apoptosis with  
that shown using the DeadEnd kit. Both TUNEL kits indicated induction of 
DNA  strand breaks after pesticide treatments and differences in apoptosis 
levels  in the tissue sections. There were variations in the distribution of  
apoptosis, which was uneven and inconsistent. ISCDDK was found to demonstrate 
 DNA-fragmentation after both apoptotic and necrotic cell death [22, 23]. 
There  were differences in apoptosis appearance in the midgut and apoptotic 
cells  were  observed randomly in the  epithelium of pesticide-treated 
larvae. Normal apoptotic cell death level in  the epithelium observed in both 
groups of control larvae (untreated diet and  acetone treated diet) was ~10%. 
Observed elevated death rates in the midgut  columnar cells and in ovarian 
or salivary gland cells of pesticide treated  larvae may be triggered by an 
apoptotic pathway after pesticide application.  All applied pesticides 
induced significant apoptotic cell death in the larvae  midgut as demonstrated 
through the use of both TUNEL kits. Necrosis, which  usually is caused by a 
lethal accident or disease opposed to a programmed  process, can be detected by 
TUNEL as found in Orita et al. [33]  and in previous experiments where 
larvae were water-treated [10].   
Interestingly,  fluvalinate resulted in the lowest levels of observed cell 
death of any  pesticide treated larvae. Fluvalinate has been used in the 
U.S.  for over two decades to control Varroa  destructor Anderson and Trueman, 
the varroa mite. Our data suggest that  honey bee larvae may have developed 
some level of resistance to fluvalinate  exposure. Equally interesting is 
that the herbicides glyphosate and simazine  and fungicides myclobutanil and 
chlorothalonil induced elevated apoptotic cell  death in an insect. Though 
unclear how this may affect honey bees at the  individual organism or colony 
level, the data suggest that herbicides and  fungicides cannot be presumed 
innocuous to bees. Regardless, the level of  stress-induced apoptosis related 
to pesticide treatment in bee larvae in our  experiment was comparable to 
that experienced by two invasive bivalves exposed  to a molluscicide [35]. 
In  our experiment, the tested insecticides, fungicides and herbicides 
induced  elevated level of apoptosis in the larval midgut. In previous 
experiments,  lower concentrations of coumaphos applied to adult worker bees did not 
trigger  increased levels of apoptosis in hypopharyngeal glands compared to 
that in  untreated bees [20].  In contrast, honey bee larvae treated with 
acaricides experienced apoptosis  and stress-induced, necrotic cell deletion 
[10],  indicating that these different types of cell death can occur 
simultaneously  after exposure to pesticides [32].   
Follicular  maturation during oogenesis involves necrosis along with 
apoptosis  [36]  and investigators have shown that necrosis potentially can 
accompany apoptosis  during normal development as shown in experiments with mouse 
cell embryos  [37].  Thus, necrotic and apoptotic cell death often occur 
simultaneously during many  pathological processes, as seen in the present 
study, and during normal  processes such as tissue renewal, embryogenesis, and 
immune response.   
In  our study, we confirmed elevated levels of apoptosis in larvae treated 
with  pesticides. The epithelial cell nuclei remained morphologically 
unchanged but  became TUNEL-positive, indicating that the DNA was fragmented but 
not  different from neighboring cell nuclei otherwise. It is possible that 
the  induced larval cell apoptosis trigged by pesticide treatment in our study 
may  have been a reversible process in the midgut tissue, one from which 
the  affected larvae could recover. On the other hand, the appearance of 
apoptosis  may precede further tissue deletion, the development of necrosis in 
the midgut  cells, or cell death altogether. The TUNEL method thus is a useful 
diagnostic  tool to monitor subclinical changes in honey bee larvae induced 
by external  influences. 
The  apoptosis of regenerative cells observed in the basal area of the 
epithelium  of pesticide treated larvae may function to maintain the proper 
ratio of cells  in the midgut, i.e. large numbers of regenerative cells may die 
to compensate  for the inadequate number of epithelial cells. This apoptotic 
mechanism has  been suggested for Drosophila cell  mechanisms which cause 
dying germline and follicle cells in Drosophila ovaries [38].  Other 
investigators observed that the percentage of epithelial cells labeled  with 
digoxigenin using the ISCDDK increased to 70% in 3-day-old larvae when to  the 
larvae were treated with formic acid [39].  The high cell death levels detected 
using ISCDDK likely indicated accidental  cell death leading to necrosis, 
triggered by necrotic injury [39].  Further studies should be performed to 
establish whether higher pesticide  concentrations can decrease apoptosis and 
increase necrosis in honey bee  larvae and how this may affect clinical 
symptoms or larvae mortality.   
Our data indicate that Annexin V has a widespread distribution in  
pesticide treated larvae being found in the midgut epithelium, salivary glands  and 
ovaries. Microscopic analyses on cellular localization of Annexin V would  
help to obtain information on its function. Intracellular and extracellular  
localizations of Annexin V have been reported in human cardiac muscle and 
vary  based on changes in disease states [40].  It has also been reported that 
in the ischemic rat heart, Annexin V leaked  from cardiac cells into the 
extracellular space and that the cardiac cell  membrane was stained intensely 
by the anti-Annexin V antibody [41].  In our study, the varied localization 
of Annexin V suggests that this protein  is related closely to apoptotic 
cell death in tissues of bee larvae exposed to  pesticides. These findings may 
contribute to a better understanding of  potential cell injury during and 
after pesticide exposure, especially due to  the possibility of 
false-negatives produced using TUNEL kits [28].  Moreover,  cell death detection and 
quantification can be more accurate and potential  artifacts can be reduced by 
using more than one assay [25].  
Collectively,  our data indicate that the nine test pesticides can induce 
apoptosis in  tissues of honey bee larvae reared in an incubator. The data 
also suggest that  the pesticide doses we tested were tolerable to larvae 
because apoptosis  likely was initiated as a protective mechanism in the midgut, 
salivary glands  or ovaries, though further expansion into necrosis, tissue 
deletion and larval  death is a potential development of these events. 
Future studies will be  necessary to explore the effects and modes of action of 
different doses of  these pesticides on larvae at the cellular and tissue 
levels. The  quantification of cell death could be used to monitor the 
subclinical and  sub-lethal effects of applied pesticides on larval tissue. Honey 
bee larvae  reared in vitro could be used in  the future as models for 
studying the effects of chemicals on living tissues  at the cellular level. 
Acknowledgements   
We  would like to thank Jeanette Klopchin and Michelle Kelley (University 
of  Florida Honey Bee  Research and Extension Laboratory) for their  
technical assistance with this project. We also thank Catherine Zettel Nalen  (UF 
HBREL) for editing an earlier draft of the manuscript and Michael Scharf  (UF 
Department of Entomology and Nematology) for assistance with pesticide  
dosing. We would like to thank Prof. Dr.  Elaine C. M. Silva-Zacarin 
(Universidade Federal de Sa˜o Carlos  (UFSCar), Campus Sorocaba, Brazil) for reading  
the manuscript and useful   suggestions. This work was supported by the 
National Honey Board  and the Florida Department of Agriculture and Consumer 
Services through the  work of the Honey Bee Technical Council.  

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Table 1.  Mortality in the  midgut columnar cells determined using two 
TUNEL kits, DeadEnd and  ISCDDK. Data are mean ± s.e. proportion cells 
positively stained, N out  of at least 300 cells counted from a minimum of 3 larvae. 
When both  treatments were analyzed together, neither technique (DeadEnd or 
ISCDDK  - F = 1.1; df = 1,123; P = 0.29) nor the interaction  between 
technique and treatment (F = 1.6; df = 10,123; P = 0.13) affected the  proportion 
of cells positively stained. Data in columns followed by the  same letter 
are not different at P < 0.05. Students T tests  were used to compare means.   
 
Type of  pesticide  
Treatment  ↓  
Dead End  technique  
ISDDK  technique  
Both techniques  analyzed together   
Insecticide  
Chlorpyrifos    
0.56 ± 0.08,  6abc  
0.74 ± 0.04,  6a  
0.65 ± 0.05,  12abc   
Imidacloprid  
0.51 ± 0.12,  6bcd  
0.76 ± 0.02,  4a  
0.61 ± 0.08,  10abc   
Amitraz*  
0.64 ± 0.07,  5abc  
0.37 ± 0.03,  4c  
0.52 ± 0.06,  9c   
Fluvalinate*  
0.29 ± 0.04,  7d  
0.32 ± 0.02,  3c  
0.30 ± 0.03,  10d   
Coumaphos*  
0.58 ± 0.12,  8abc  
0.48 ± 0.03,  5bc  
0.54 ± 0.07,  13c 
Fungicide  
Myclobutanil  
0.62 ± 0.11,  5abc  
0.78 ± 0.06,  4a  
0.69 ± 0.07,  9ab   
Chlorothalonil  
0.49 ± 0.08,  7cd  
0.66 ± 0.06,  4ab  
0.55 ± 0.06,  11bc 
Herbicide  
Glyphosate  
0.74 ± 0.05,  5ab  
0.65 ± 0.15,  5a  
0.69 ± 0.08,  10ab   
Simazine  
0.76 ± 0.06,  7a  
0.77 ± 0.06,  7a  
0.77 ± 0.04,  14a 
Control  
Diet with  acetone  
0.10 ± 0.01,  8e  
0.11 ± 0.03,  5d  
0.11 ± 0.01,  13e   
Diet  only  
0.10 ± 0.02,  8e  
0.09 ± 0.02,  5d  
0.10 ± 0.02,  13e 
ANOVA→  
F = 10.6; df =  10,71; P <  0.01  
F = 16.3; df =  10,51; P <  0.01  
Treatment  effect: F = 22.2; df =  10,123; P <  0.01   
*Used in honey  bee colonies to control varroa  mites
Figure  1. Staining  of formalin-fixed, paraffin-embedded larvae on which 
the DeadEnd colorimetric  apoptosis detection system (Promega, Madison, WI,  
USA) was used.  Larvae were 6 d old, 24 h after the last of four consecutive 
daily pesticide  treatments and prepared for immunohistology. Peroxidase 
conjugated  anti-digoxigenin secondary antibody and DAB as a substrate were 
used to obtain  a specific brown reaction product. The  DAB reaction product 
localized to the nuclei of the columnar midgut epithelial  cells is indicated 
by black arrows and the DAB reaction product localized to  the regenerative 
cells is indicated by a black arrow head. When the DAB  reaction product is 
absent, either the arrow (columnar midgut epithelial  cells) or arrow head 
(regenerative cells) is white. Panel 1A  shows  the midgut, of a 
simazine-treated larva. The DAB reaction product is localized  to the nuclei of the 
most  of the epithelial columnar  and regenerative cells. Panel B shows 
chlorpyrifos treated larva with the DAB  reaction product localized to the 
regenerative epithelial cells but not the  columnar ones. Panel C shows an amitraz 
treated larva where the DAB reaction  product was localized in columnar and 
regenerative epithelial cells.  Panel  D shows sections of the midgut of an 
imidacloprid treated larva with the DAB  reaction product localized in the 
nuclei of columnar cells  but not in  regenerative cells. Panel E shows a 
chlorothalonil treated larva. The DAB  reaction product was found sporadically 
in the migut columnar epithelial  cells. Panel F shows an untreated larva 
where only ~10 % DAB positive midgut  epithelial cells were found. Panel G 
shows an amitraz treated larva where DAB  positive and negative salivary glands 
cells  were seen.  Panel H shows an imidacloprid treated larva with 
indicative DAB staining in  ovariole nurse cells. Panel I shows a control larva 
where the DAB reaction was  distributed sporadically in ovariole nurse cells. 
Panel J shows a control  section of an imidacloprid treated larva where 
endogenous peroxidase was  quenched successfully and enzyme incubation was 
omitted. No DAB reaction  product was found. Magnification of all panels: 400×. 

Figure  2. Sections  of formalin-fixed, paraffin-embedded, 6 d old larvae, 
24 h after the last of  four consecutive daily pesticide treatments. Cell 
death was detected using the  TUNEL technique ISCDDK (Roche). TdT-mediated 
dUTP for DNA labeling was  employed, followed by the application of 
anti-fluorescein alkaline phosphatase  conjugated antibody, using fast red for 
visualization, and counterstaining  with haematoxylin. Dense red azo dye staining 
localized to the nuclei of the  midgut epithelial cells, in the salivary gland 
cells, or in ovary nurse cells  indicative of impending cell death is 
indicated  by a black arrow. Reaction product localization to the regenerative 
cells is  indicated by a black arrow head. Where the reaction product is 
absent, either  the arrow (midgut epithelial cells) or arrow head (regenerative 
cells) is  white. Panel  A shows a chlorpyrifos-treated larva with red azo 
dye staining localized to  the midgut columnar epithelial-cell nuclei  but not 
the regenerative epithelial cells. Panel  B shows midgut epithelium in a 
simazine-treated larva. The Red azo-dye  reaction product localized to the 
columnar and regenerative cells. Panel C  shows a midgut epithelium section of 
a coumaphos-treated larva. The Red  azo-dye reaction product localized to 
the columnar  and  regenerative  epithelial  cells. Panel D shows salivary 
gland tissue of a myclobutanil-treated larva  where the majority of cells were 
alkaline phosphatase positive.  Panel E shows untreated,  control larvae 
with red azo-dye reaction product to sporadic salivary gland  cells. Panel F 
shows the red azo-dye product sporadically in nurse cells in  ovaries of a 
simazine-treated larva. Magnification of all panels:  400×. 

Figure  3. Immunohistochemical  localization of AnnexinV cells of 
formalin-fixed,  paraffin-embedded 6 d old larvae, 24 h after the last of four 
consecutive  daily pesticide treatments.  
Panel  A shows the red azo-dye reaction product bound to the apical brush 
border  (black  arrow) in  a chlorpyrifos-treated larva. The reaction product 
was not localized in the  midgut cells (white  arrow head).  Panel B shows 
cells from a glyphosate-treated larva and indicates Annexin V  staining 
throughout the remaining midgut epithelium cytoplasm (black  arrow). Panel  C 
shows a midgut section of a glyphosate-treated larva with red azo-dye  
staining indicating PS localized to the basal and apical cell cytoplasm  (black  
arrow head).  Panel D indicates that an alkaline phosphatase reaction product 
in a  simazine-treated larva was localized to the cytoplasm of the columnar 
cells at  the basal area (black  arrow head).  Panel E shows red azo-dye 
localized in the salivary gland tissue of a  myclobutanil-treated larva (black 
arrow head). Panel F shows a  glyphosate-treated larva in which red azo-dye 
was localized to ovarian nurse  cells (black  arrow head).  Panel G shows no 
intensive staining in the salivary gland tissue of a larva  consuming 
untreated food. Panel H shows cells from an untreated, control larva  with red 
azo-dye reaction product to some sections of the midgut epithelium  bound to 
the apical and basal cell membrane (black  arrow head).  The cell cytoplasm 
of the midgut cells was not stained. Magnification of all  panels: 400×. 


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